CN101412705A - Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound - Google Patents

Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound Download PDF

Info

Publication number
CN101412705A
CN101412705A CN 200810122251 CN200810122251A CN101412705A CN 101412705 A CN101412705 A CN 101412705A CN 200810122251 CN200810122251 CN 200810122251 CN 200810122251 A CN200810122251 A CN 200810122251A CN 101412705 A CN101412705 A CN 101412705A
Authority
CN
Grant status
Application
Patent type
Prior art keywords
yue
propyl
propanediol
amine catalyst
methyl
Prior art date
Application number
CN 200810122251
Other languages
Chinese (zh)
Inventor
李坚军
苏为科
通 蒲
金林勇
Original Assignee
浙江工业大学;浙江车头制药有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date

Links

Abstract

The invention relates to a method for synthesizing a 2-methyl-2-propyl-1, 3-propanediol diester carbonate compound by using trichloromethyl chloroformate, which comprises the following steps: using 2-methyl-2-propyl 1, 3-propanediol and the trichloromethyl chloroformate as raw materials to completely react with each other under the action of an organic amine catalyst in an organic solvent at a temperature of between 5 DEG C below zero and 50 DEG C, and separating and purifying reaction solution to obtain the 2-methyl-2-propyl-1, 3-propanediol diester carbonate, wherein the molar ratio of the 2-methyl-2-propyl 1, 3-propanediol to the trichloromethyl chloroformate to the organic amine catalyst is 1 to 0.5-2.5 to 0.2-2.5. The method adopts the trichloromethyl chloroformate to prepare the key intermediate 2-methyl-2-propyl-1, 3-propanediol diester carbonate of carisoprodol, has high yield, safety, no pollution, and simple operation and is a synthetic route with broad industrialization prospect.

Description

2-曱基-2-丙基-1, 3-丙二醇碳酸二酯化合物的合成方法(一)技术领域 2- Yue-2-propyl-1, 1,3-propanediol synthesis of carbonic diester compound (a) Technical Field

本发明涉及一种2-甲基-2-丙基-l, 3-丙二醇碳酸二酯的合成方法。 The present invention relates to a 2-propyl -l, 1,3-propanediol synthesis of carbonic acid esters.

(二) 背景技术 (B) Background Art

2-曱基-2-丙基-l, 3-丙二醇碳酸二酯是卡利普多的关键中间体, 卡利普多也称卡立普多,是美国二十世纪六十年代开发的中枢性骨骼月/L^弛药,收载于美国药典(27版),主要生产地为瑞士、意大利、 印度,近年来在美国药品市场销售额逐渐上升的销售势头:2000、 2001, 2002年在美国200个畅销通用名药排行榜中排名分别位第26、 28, 24位,相对应的销售额分别为1. 82、 2.31和丄8亿元美元。 2- Yue-2-propyl -l, 3- propylene carbonate diester is more Galip key intermediate, also known as multi Galip carisoprodol, US nineteen sixties developed hub skeletal month / L ^ relaxation drugs, contained in a United States Pharmacopeia (27th edition), the main production for Switzerland, Italy, India, in recent years in the US pharmaceutical market sales gradually rising sales momentum: in 2000, 2001, 2002 United States 200 best-selling generic drugs rankings were ranked No. 26, 28, 24, the corresponding sales were 1.82, 2.31 and Shang US $ 800 billion. 专家预测,到2010年,全球这一市场的销售额预计将超过400亿美元。 Experts predict that by 2010, global sales of this market is expected to exceed $ 40 billion.

在本发明给出之前,该产品一般通过光气法来合成,虽然光气法合成氨曱酸酯类药物在技术上已经成熟,但是,在光气(C0Cl2)法工业生产过程中,对反应设备密封性要求很高,投资也较大,尾气中的光气从环保角度看会带来很大麻烦。 Prior to the present invention are given, the product is generally synthesized by the phosgene method, the phosgene method although ammonia Yue esters technically mature drugs, however, in the industrial production of phosgene (C0Cl2) process method, the reaction apparatus tightness demanding, investment is large, light gas exhaust from the environmental point of view will bring a lot of trouble. 在生产上必须多一套生产和贮存光气的设备而且过程仍然存在很大的安全隐患。 We must be more than a set of production and storage of phosgene in the production of equipment and process there is a big security risk.

(三) 发明内容 (Iii) Disclosure of the Invention

本发明的目的是提供一种工艺简单,生产安全稳定可靠、反应收率高、成本低、基本无三废的2-甲基-2-丙基-1, 3-丙二醇碳酸二酯的合成方法。 Object of the present invention is to provide a simple process, the production of safe and reliable, high reaction yield, low cost and substantially no waste methyl-2-propyl-1, 1,3-propanediol synthesis of carbonic acid esters.

本发明采用的技术方案如下: The present invention adopts the following technical solution:

一种如式(I )所示的2-甲基-2-丙基-1, 3-丙二醇碳酸二酯化合物的合成方法,以式(II )所示的2-曱基-2-丙基-1, 3-丙二醇和氯曱酸三氯曱酯为原料,在有机胺催化剂作用下在有机溶剂中于-5 ~ 5(TC反应完全,反应液分离纯化即得所述的2-曱基-2-丙基-l, 3-丙二醇碳酸二酯,所述的2-甲基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酉旨:有机胺催化剂物质的量比为1: 0.5-2.5: 0.2-2.5; Methyl-2-propyl-1, 1,3-propanediol synthesis of carbonic diester compound, 2- Yue group in formula (II) -2-propyl-A shown in formula (I) shown in FIG. -1-chloro-1,3-propanediol and Yue Yue acid trichloromethyl ester as raw materials, at -5 ~ 5 (TC completion of the reaction, 2-Yue-based separation to obtain the reaction solution was treated in an organic solvent in the presence of an organic amine catalyst 2-propyl -l, 1,3-propanediol diester carbonate, the 2-propyl-1,3-propanediol: Yue-chloro-trichloro acid Yue unitary purpose: ratio of organic amine catalyst material is 1: 0.5-2.5: 0.2-2.5;

OH OH

所述的投料物质的量比优选为2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂1: 0. 55~2.0: 0. 2 ~ 2. 0。 The ratio of the feed material is preferably 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: an organic amine catalyst 1: 0.55 to 2.0: 0.2 to 2 0.

本发明是以气相色谱跟踪监测反应,来判定反应终点。 The present invention is based on tracking and monitoring the reaction by gas chromatography, to determine the end of the reaction. 通常需要4~20小时才能反应完全。 Usually it takes 4 to 20 hours to complete the reaction.

本发明所述的有机溶剂为下列之一或一种以上的任意比例的混合物:C1〜C5的卣代烷烃、C1〜C8的脂肪酯、C3-C8的酮、C2 ~ C8 的醚。 The present invention is an organic solvent mixture in any ratio or one or more of the following: alkanes C1~C5 the wine container, C1~C8 fatty esters, C3-C8 ketones, C2 ~ C8 ether. 或者所述的有机溶剂为下列之一或一种以上的任意比例的混合物:苯、曱苯、二曱苯、氯苯、硝基苯、环己烷、二硫化碳或硝基曱烷。 The organic solvent or a mixture in any ratio or one or more of the following: benzene, Yue benzene, Yue benzene, chlorobenzene, nitrobenzene, cyclohexane, carbon disulfide Yue alkoxy or nitro. 所述的有机溶剂优选为下列之一或一种以上任意比例的混合物: 二氯曱烷、三氯曱烷、四氯化石友、1, 1-二氯乙烷、1, 2-二氯乙烷、1,1, 1-三氯乙烷或1,1,2-三氯乙烷、乙酸曱酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酸异丙酯、乙酸异丁酯、乙酸戊酯、乙酸异戊酯、丙酸曱酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸戊酯、丙酮、丁酮、环己酮、乙醚、丙醚、异丙醚、丁醚、四氢呋喃或苯、甲苯、二曱苯、氯苯、硝基苯、环己烷、二硫化碳或硝基曱烷。 The organic solvent is preferably one or more of the following, or an arbitrary mixture ratio: Yue-dichloro alkyl, alkoxy trichloromethyl Yue, tetrachlorophthalic fossil Friends, 1, 1-dichloroethane, 1,2-dichloroethane alkyl, 1,1,1-trichloroethane or 1,1,2-trichloroethane, Yue acetate, ethyl acetate, propyl acetate, butyl acetate, isopropyl acetate, isobutyl acetate, amyl acetate, isoamyl acetate, propionate, Yue acetate, ethyl propionate, propyl propionate, butyl propionate, amyl acetate, acetone, methyl ethyl ketone, cyclohexanone, diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, tetrahydrofuran or benzene, toluene, diethyl Yue benzene, chlorobenzene, nitrobenzene, cyclohexane, carbon disulfide Yue alkoxy or nitro. 本发明所用有机溶剂更优选为下列之一:乙酸曱酯、乙酸乙酯、苯、氯苯、曱苯、环己烷、 环己酮、二氯曱烷、1, 2-二氯乙烷、氯仿或四氯化碳。 The organic solvent used in the present invention is more preferably one of the following: Yue acetate, ethyl acetate, benzene, chlorobenzene, Yue benzene, cyclohexane, cyclohexanone, Yue-dichloro-dioxane, 1,2-dichloroethane, chloroform or carbon tetrachloride. 本发明方法中有机溶剂的总用量为2-曱基-2-丙基-l,3-丙二醇质量的2~20倍, 优选2〜15倍。 The method of the present invention, the total amount of organic solvent is 2-Yue-2-propyl -l, 2 ~ 20 times the mass of 1,3-propanediol, preferably 2~15 times.

进一步,所述的有机胺催化剂为下列之一或一种以上任意比例的混合物:N,N-二曱基苯胺,吡啶,哌啶,N,N-二曱基曱酰胺,N, N-二曱基乙酰胺,三乙胺,1, 3-二曱基咪唑烷酮,N-曱基四氢吡咯, 四曱基胍,四曱基脲,N, N-二丁基曱酰胺或N-曱基吗啉,优选下列之一:1, 3-二曱基-2-咪唑烷酮、三乙—胺、N,N-二曱基曱酰胺或吡啶。 Further, the organic amine catalyst is one of the following or a mixture in any ratio above: N, N- two Yue aniline, pyridine, piperidine, N, N- two Yue Yue amide group, N, N- two Yue acetamide, triethylamine, 1, 3-Yue imidazolidinone, N- Yue pyrrolidine group, four Yue guanidine, tetra Yue urea, N, N- dibutyl amide or N- Yue Yue morpholine, preferably one of the following: 1, 3-Yue-2-imidazolidinone, triethyl - amine, N, N- two Yue Yue amide group or pyridine.

本发明是以气相色谱跟踪监测反应,反应完全后,反应液加水, 分离取有机层,回收溶剂,即得所述的2-曱基-2-丙基-1, 3-丙二醇 The present invention is based on tracking and monitoring the reaction by gas chromatography, after completion of the reaction, the reaction solution was added water, the organic layer was separated, the solvent was recovered to obtain the 2-Yue-2-propyl-1,3-propanediol

碳酸二酯。 Carbonic acid diester.

具体的,所述的2-曱基-2-丙基-1, 3-丙二醇碳酸二酯化合物的合成方法按照以下步骤进行:按照2-曱基-2-丙基-1, 3-丙二醇:有机胺催化剂的物质的量比为1: 0.2-2.0投料,加入有机溶剂溶解, 然后緩慢滴加溶有物质的量为2-曱基-2-丙基-1, 3-丙二醇0.55-2. 0倍的氯曱酸三氯曱酯的有机溶剂的溶液,滴加完毕后在-5 ~ 50°C 反应10~ 20小时至反应完全,反应液加水,分离取有4几层,回收溶剂,即得所述的2-曱基-2-丙基-l, 3-丙二醇碳酸二酯。 Specifically, the 2-Yue-2-propyl-1, 1,3-propanediol synthesis of carbonic diester compound is carried out according to the following steps: according to 2- Yue-2-propyl-1,3-propanediol: the molar ratio of organic amine catalyst is 1: 0.2-2.0 feed, adding an organic solvent to dissolve, and then the amount of material dissolved slowly added dropwise to 2- Yue-2-propyl-1,3-propanediol 0.55-2. 0 times the organic solvent solution of the acid chloride Yue Yue trichlorophenyl ester, after the addition was complete the reaction at 10 to 20 hours to -5 ~ 50 ° C the reaction was complete, the reaction solution was added water, separating the layers take 4, recovery of the solvent, Yue obtain the 2-2-propyl -l, 3- propylene carbonate diester. 所述的有机胺催化剂为1, 3-二甲基-2-咪唑烷酮、三乙胺、N,N-二曱基曱酰胺或吡咬,所述的有机溶剂为乙酸乙酯或环己酮或氯仿,所加入有机溶剂总的质量为2-曱基-2-丙基-l, 3-丙二醇的2 ~ 15倍。 The organic amine catalyst is 1,3-dimethyl-2-imidazolidinone, triethylamine, N, N- two Yue Yue amide group or pyrazolyl bite, said organic solvent is ethyl acetate or cyclohexyl ketone, or chloroform, is added to the total mass of the organic solvent is 2 Yue-2-propyl -l, 2 ~ 15 times of 1,3-propanediol.

本发明与现有技术相比,其有益效果体现在: Compared with the prior art the present invention, which is reflected in the beneficial effects:

从根本上消除了传统工艺安全隐患大、三废污染严重等问题。 Eliminating the traditional process of security risk, a serious waste pollution problem fundamentally. 具有安全、三废少,能耗小,总收率高,成本低、质量优等优点。 Safe, less waste, low energy consumption, high total yield, low cost, excellent quality advantages.

(四)具体实施方式: (IV) DETAILED DESCRIPTION:

以下以具体实施例来说明本发明的技术方案,但本发明的保护范围不限于此: 实施例1 The following specific examples will be described in the technical solutions of the present invention, but the scope of the present invention is not limited thereto: Example 1

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 2投料,2-甲基-2-丙基-1, 3-丙二醇30 g;氯曱酸三氯曱酯22. 46 g;有机溶剂氯苯120 g;有机胺催化剂为N, N-二曱基苯胺,投料质量5.49 g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.2 feed, 2-methyl-propyl yl-1,3-propanediol 30 g; acid chloride Yue Yue trichlorophenyl ester 22. 46 g; chlorobenzene organic solvent 120 g; the organic amine catalyst is N, N- two Yue aniline, feed mass 5.49 g;

将2-曱基-2-丙基-1, 3-丙二醇和有机胺催化剂溶解于部份有机溶剂中,降温至-5~15°C,緩慢滴加以少量有机溶剂溶解的氯曱酸三氯曱酯溶液,滴加完毕后在50。 2- Yue-2-propyl-1,3-propanediol and organic amine catalyst is dissolved in an organic solvent partially, cooled to -5 ~ 15 ° C, was slowly dropwise trichloromethyl be an acid chloride Yue small amounts of organic solvent soluble Yue ester solution, at 50 after completion of the dropwise addition. C进行反应,用气相色谱跟踪监测反应终点,直至反应完毕,用于溶解2-曱基-2-丙基-1, 3-丙二醇和有机胺催化剂的氯苯与用于溶解氯曱酸三氯曱酯的有机溶剂氯苯的总量为120 g。 C reaction, the end of the reaction was monitored by gas chromatography track, until completion of the reaction for dissolving 2- Yue-2-propyl-1,3-propanediol and organic amine catalyst is used to dissolve chlorine Yue chlorophenyl trichloro acid the total amount of organic solvent is chlorobenzene Yue ester is 120 g.

反应完毕后,反应液加入反应液一倍量的水,分层,分离除去水, 取有机层,回收溶剂,即得卡利普多关键中间体2-曱基-2-丙基-1, 3-丙二醇碳酸二酯26. 93g,收率75. 0%,纯度98. 0%。 After completion of the reaction, the reaction solution was added twice amount of the reaction water, layers were separated, the water separated was removed, the organic layer, the solvent was recovered to obtain a key intermediate 2 Galip plurality Yue-2-propyl-1, 1,3-propanediol carbonate diester 26. 93g, 75.0% yield, 98.0% purity. 实施例2 Example 2

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 5投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22. 46g;有机溶剂氯苯120g;有机胺催化剂为N, N-二曱基苯胺,投料质量13. 73g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.5 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22. 46g; 120g organic solvent chlorobenzene; an organic amine catalyst is N, N- two Yue aniline, feed mass 13. 73g;

反应在3(TC温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯25. 20g,收率70. 2%,纯度98. 1%。 实施例3 Reaction is carried out (at temperature TC 3, other steps according to Example L, Yue give 2-2-propyl -1, 25. 20g 3- propylene carbonate diester, yield 70.2%, purity 98.1 %. Example 3

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.7: 0. 5投料,2-甲基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯31.45g;有机溶剂环己酮180 g;有机胺催化剂为N, N-二曱基苯胺,投料质量13. 73g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.7: 0.5 feed, 2-methyl-propyl yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 31.45g; organic solvent cyclohexanone 180 g; the organic amine catalyst is N, N- two Yue aniline, feed mass 13. 73g;

反应在-5。 Reaction at -5. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 07g,收率82. 1%,纯度98. 1%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 28. 07g, 82. 1% yield, 98.1% purity. 实施例4 Example 4

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.7: 0. 8投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯31. 45g;有机溶剂环己酮180 g;有机胺催化剂为N, N-二曱基苯胺,投料质量21.97g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.7: 0.8 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 31. 45g; organic solvent cyclohexanone 180 g; the organic amine catalyst is N, N- two Yue aniline, 21.97 g feed quality;

反应在20。 In reaction 20. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯29. 47g,收率82. 1%,纯度98. 1%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 29. 47g, 82. 1% yield, 98.1% purity. 实施例5 Example 5

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 1.0: 1.0投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯44. 93g;有机溶剂环己酮180 g;有机胺催化剂为N, N-二曱基苯胺,投料质量27. 46g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 1.0: 1.0 feeding, 2- Yue-2-propyl - 1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 44. 93g; organic solvent cyclohexanone 180 g; the organic amine catalyst is N, N- two Yue aniline, feed mass 27. 46g;

反应在4(TC温度下进行,其它操:作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 72g,收率83. 2%,纯度97. 8%。 实施例6 Reaction is carried out (at temperature TC 4, other operations: the same embodiment as in Example l, to give 2-2-propyl Yue -1, 28. 72g 3- propylene carbonate diester, yield 83.2%, purity 97 8% Example 6

按照2-曱基-2-丙基-l, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 1.0: 0. 2投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯甲酯44. 93g;有机溶剂乙酸正丁酯180 g;有机胺催化剂为吡啶,l殳^h质量3. 59g; According 2- Yue-2-propyl -l, 3- propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 1.0: 0.2 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; Yue acid chloride trichloromethyl 44. 93g; organic solvent is n-butyl acetate 180 g; organic amine catalyst is pyridine, l ^ h Shu mass 3. 59g;

反应在(TC温度下进行,其它操作同实施例1,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯21. 97g,收率61.2%,纯度97. 5%。 实施例7按照2-曱基-2-丙基-l, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 1.0: 0. 4投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯44. 93g;有机溶剂乙酸正丁酯180 g;有机胺催化剂为吡啶,投料质量7. 17g; Reaction is carried out (at temperature TC, other operation is the same as in Example 1 to give 2 Yue-2-propyl-1,3-propanediol carbonate diester 21. 97g, 61.2% yield, 97.5% purity. Embodiment Example 7 2- Yue-2-propyl -l, 3- propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 1.0: 0.4 feed, 2-2 Yue - propyl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 44. 93g; organic solvent is n-butyl acetate 180 g; organic amine catalyst is pyridine, feed quality 7. 17g;

反应在50。 In reaction 50. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯25. 96g,收率72. 3%,纯度97. 8%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 25. 96g, 72. 3% yield, 97.8% purity. 实施例8 Example 8

按照2-曱基-2-丙基-l, 3-丙二醇:氯曱酸三氯甲酯:有机胺催化剂物质的量比为1: 1.0: 0. 6投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯44. 93g;有机溶剂乙酸正丁酯180 g;有机胺催化剂为吡啶,投料质量IO. 76g; According 2- Yue-2-propyl -l, 3- propanediol: Yue-chloro-trichloromethyl acid: organic amine catalyst ratio was 1: 1.0: 0.6 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 44. 93g; organic solvent is n-butyl acetate 180 g; organic amine catalyst is pyridine, feed quality IO 76g.;

反应在20。 In reaction 20. C温度下进行,其它操作同实施例l,得2-甲基-2-丙基-1, 3-丙二醇碳酸二酯25. 13g,收率70.0%,纯度98. 0%。 C conducted at a temperature, other operations as in Example L, to give 2-propyl-1,3-propanediol carbonate diester 25. 13g, 70.0% yield, 98.0% purity. 实施例9 Example 9

按照2-曱基-2-丙基-1, 3-丙二醇:氯甲酸三氯曱酯:有机胺催化剂物质的量比为1: 1.0: 0. 8投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯44. 93g;有才几溶剂乙醚180 g;有机胺催化M 为吡啶,投料质量14. 34g; According 2- Yue-2-propyl-1,3-propanediol: Yue trichloromethyl chloroformate ester: organic amine catalyst ratio was 1: 1.0: 0.8 feeding, Yue-2-propyl 2- -1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 44. 93g; talented several solvent such as ether 180 g; M organic amine catalyst is pyridine, feed mass 14. 34g;

反应在回流温度下进行,其它操作同实施例1,得2-甲基-2-丙基-l, 3-丙二醇碳酸二酯27. 00g,收率75. 1%,纯度97. 8%。 The reaction is carried out at reflux temperature, the other operation is the same as in Example 1 to give 2-propyl -l, 3- propylene carbonate diester 27. 00g, 75.1% yield, 97.8% purity. 实施例10 Example 10

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯甲酯:有机胺催化剂物质的量比为1: 1.5: 1.0投料,2-甲基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯67. 40g;有机溶剂曱苯180 g;有机胺催化剂为吡啶,投料质量17. 93g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichloromethyl acid: organic amine catalyst ratio was 1: 1.5: 1.0 feed, 2-methyl-2-propyl - 1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 67. 40g; benzene organic solvent Yue 180 g; organic amine catalyst is pyridine, feed mass 17. 93g;

反应在20。 In reaction 20. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-l, 3-丙二醇碳酸二酯29. 08g,收率81.0%,纯度98. 2%。 C conducted at a temperature of, for example, the same operations other embodiments l, Yue give 2-2-propyl -l, 3- propylene carbonate diester 29. 08g, 81.0% yield, 98.2% purity. 实施例11 Example 11

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 1.5: 1.6投料,2-甲基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯67. 40g;有机溶剂1, 2-二氯乙烷180g;有机胺催化剂为吡啶,投料质量28. 68g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 1.5: 1.6 feed, 2-methyl-2-propyl - 1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 67. 40g; organic solvent 1, 2-dichloroethane 180g; organic amine catalyst is pyridine, feed mass 28. 68g;

反应在-3。 The reaction -3. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 33g,收率78. 9%,纯度98. 2%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 28. 33g, 78. 9% yield, 98.2% purity. 实施例12 Example 12

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 2投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22. 46g;有机溶剂丙酮180 g;有机胺催化剂为三乙胺,投料质量4. 5g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.2 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22. 46g; organic solvent acetone 180 g; the organic amine catalyst is triethylamine, feed quality 4. 5g;

反应在l(TC温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯26. 78g,收率74.6%,纯度98. 0%。 实施例13 The reaction in the l (TC temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 26. 78g, 74.6% yield, 98.0% purity. Example 13

按照2-曱基-2-丙基-l, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 4投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22.46g;有机溶剂1, 2-二氯乙烷180g;有机胺催化剂为三乙胺,投料质量9. 17g; According 2- Yue-2-propyl -l, 3- propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.4 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22.46g; organic solvent 1, 2-dichloroethane 180g; organic amine catalyst is triethylamine, feed quality 9. 17g;

反应在30。 In reaction 30. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯29. 51g,收率82. 2%,纯度98. 0%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 29. 51g, 82. 2% yield, 98.0% purity. 实施例14 Example 14

按照2-甲基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 6投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯甲酸三氯曱酯22. 46g;有机溶剂四氢呋喃180 g;有机胺催化剂为三乙胺,投料质量13. 75g; According to 2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.6 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; Yue trichloromethyl chloroformate ester 22. 46g; organic solvent such as tetrahydrofuran 180 g; the organic amine catalyst is triethylamine, feeding mass 13. 75g;

反应在3(TC温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 22g,收率78. 6%,纯度98. 4%。 实施例15 Reaction is carried out (at temperature TC 3, other steps according to Example L, Yue give 2-2-propyl -1, 28. 22g 3- propylene carbonate diester, yield 78.6%, purity 98.4 %. Example 15

按照2-曱基-2-丙基-l, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 0. 8投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯甲酯22. 46g;有机溶剂四氢呋喃180 g;有机胺催化剂为三乙胺,投料质量18. 34g; According 2- Yue-2-propyl -l, 3- propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 0.8 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; Yue acid chloride trichloromethyl 22. 46g; organic solvent such as tetrahydrofuran 180 g; the organic amine catalyst is triethylamine, feeding mass 18. 34g;

反应在30。 In reaction 30. C温度下进行,其它操作同实赫il,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 58g,收率79. 6%,纯度98. 0%。 C conducted at a temperature, other operations with real He IL, Yue give 2-2-propyl-1,3-propanediol carbonate diester 28. 58g, 79.6% yield, 98.0% purity. 实施例16 Example 16

按照2-甲基-2-丙基-l, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 1. 0投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22. 46g;有机溶剂四氢呋喃180 g;有机胺催化剂为三乙胺,投料质量22. 92g; According to 2-propyl -l, 3- propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 1.0 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22. 46g; organic solvent such as tetrahydrofuran 180 g; the organic amine catalyst is triethylamine, feeding mass 22. 92g;

反应在30。 In reaction 30. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯27. 21g,收率75. 8%,纯度98. 2%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 27. 21g, 75.8% yield, 98.2% purity. 实施例17 Example 17

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 1. 2投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22. 46g;有机溶剂苯180 g;有机胺催化剂为三乙胺,投料质量27. 50g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 1.2 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22. 46g; organic solvents such as benzene 180 g; the organic amine catalyst is triethylamine, feeding mass 27. 50g;

反应在30。 In reaction 30. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯28. 72g,收率80. 0%,纯度97. 8%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl-1,3-propanediol carbonate diester 28. 72g, 80. 0% yield, 97.8% purity. 实施例18 Example 18

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.5: 2. 5投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯22. 46g;有机溶剂氯仿180 g;有机胺催化剂为三乙胺,投料质量57. 3g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.5: 2.5 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 22. 46g; chloroform, the organic solvent 180 g; the organic amine catalyst is triethylamine, feeding mass 57. 3g;

反应在2(TC温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇石友酸二酯27. 82g,收率77. 5%,纯度98. 1%。 实施例19 Reaction is carried out (at temperature TC 2, other steps according to Example L, Yue give 2-2-propyl-1,3-propanediol diester Friends stone 27. 82g, yield 77.5%, purity 98 1% Example 19

按照2-曱基-2-丙基-1, 3-丙二醇:氯甲酸三氯曱酯:有机胺催化剂物质的量比为1: 1.2: 0. 2投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯53. 92g;有机溶剂氯仿180 g;有机胺催化剂为N, N-二曱基曱酰胺,投料质量3. 31g;反应在20。 According 2- Yue-2-propyl-1,3-propanediol: Yue trichloromethyl chloroformate ester: organic amine catalyst ratio was 1: 1.2: 0.2 feeding, Yue-2-propyl 2- -1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 53. 92g; chloroform, the organic solvent 180 g; the organic amine catalyst is N, N- two Yue Yue amide group, feed quality 3. 31g; 20 in the reaction. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-1, 3-丙二醇碳酸二酯21. 54g,收率60. 0%,纯度97. 9%。 C conducted at a temperature of, for example, the same operations other embodiments l, Yue give 2-2-propyl-1,3-propanediol carbonate diester 21. 54g, 60. 0% yield, 97.9% purity. 实施例20 Example 20

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 1.2: 0. 4投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯53. 92g;有机溶剂氯仿180 g;有机胺催化剂为N,N-二曱基曱酰胺,投料质量6. 62g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 1.2: 0.4 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; 53. 92g chloro-trichloro Yue Yue acid ester; an organic solvent such as chloroform 180 g; the organic amine catalyst is N, N- two Yue Yue amide group, feed quality 6. 62g;

反应在20。 In reaction 20. C温度下进行,其它操作同实施例l,得2-甲基-2-丙基-l, 3-丙二醇碳酸二酯27. 21g,收率75. 8%,纯度98. 1°/。 C conducted at a temperature, other operations as in Example L, to give 2-propyl -l, 3- propylene carbonate diester 27. 21g, yield 75.8%, purity 98. 1 ° /. . 实施例21 Example 21

按照2-曱基-2-丙基-1, 3-丙二醇:氯甲酸三氯甲酯:有机胺催化剂物质的量比为1: 2.0: 0. 6投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯89. 86 g;有机溶剂氯仿180 g;有机胺催化剂为N,N-二甲基甲酰胺,投料质量9. 94g; According 2- Yue-2-propyl-1,3-propanediol: trichloromethyl chloroformate: an organic amine catalyst ratio was 1: 2.0: 0.6 feed, Yue-2-propyl 2- -1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 89. 86 g; chloroform, the organic solvent 180 g; the organic amine catalyst is N, N- dimethylformamide, feed quality 9. 94g;

反应在2(TC温度下进行,其它操作同实施例l,得2-曱基_2-丙基-l, 3-丙二醇碳酸二酯25. 67g,收率71. 5%,纯度97. 8%。 实施例22 Reaction is carried out in 2 (at temperature TC, other steps according to Example L, Yue-yl _2- give 2-propyl -l, 25. 67g 3- propylene carbonate diester, yield 71.5%, purity 97.8 %. Example 22

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 2.5: 0. 8投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯112. 33g;有机溶剂氯仿180g;有机胺催化剂为N,N-二曱基曱酰胺,投料质量13. 24g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 2.5: 0.8 feed, 2-propyl-2- Yue yl-1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 112. 33g; 180g organic solvent such as chloroform; the organic amine catalyst is N, N- two Yue Yue amide group, feed mass 13. 24g;

反应在30'C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-l, 3-丙二醇碳酸二酯25. 13g,收率70. 0%,纯度98. 1%。 The reaction is carried out at a temperature of 30'C, other steps according to Example L, Yue give 2-2-propyl -l, 25. 13g 3- propylene carbonate diester, yield 70.0%, purity 98.1 %. 实施例23 Example 23

按照2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂物质的量比为1: 0.8: 1.0投料,2-曱基-2-丙基-1, 3-丙二醇30g;氯曱酸三氯曱酯35. 94g;有机溶剂苯180 g;有机胺催化剂为N,N-二曱基甲酰胺,投料质量16. 57g; According 2- Yue-2-propyl-1,3-propanediol: Yue-chloro-trichlorophenyl ester Yue acid: organic amine catalyst ratio was 1: 0.8: 1.0 feeding, 2- Yue-2-propyl - 1, 1,3-propanediol 30g; chloro Yue Yue acid trichloromethyl ester 35. 94g; organic solvents such as benzene 180 g; the organic amine catalyst is N, N- two Yue formamide, feed mass 16. 57g;

反应在25。 In reaction 25. C温度下进行,其它操作同实施例l,得2-曱基-2-丙基-l, 3-丙二醇碳酸二酯29. 43g,收率82. 0%,纯度98. 2%。 C conducted at a temperature, other operations as in Example L, Yue give 2-2-propyl -l, 3- propylene carbonate diester 29. 43g, 82. 0% yield, 98.2% purity.

Claims (10)

  1. 1. 一种如式(I)所示的2-甲基-2-丙基-1,3-丙二醇碳酸二酯化合物的合成方法,以式(II)所示的2-甲基-2-丙基-1,3-丙二醇和氯甲酸三氯甲酯为原料,在有机胺催化剂作用下在有机溶剂中于-5~50℃反应完全,反应液分离纯化得所述的2-甲基-2-丙基-1,3-丙二醇碳酸二酯,所述的2-甲基-2-丙基-1,3-丙二醇:氯甲酸三氯甲酯:有机胺催化剂物质的量比为1:0.5~2.5:0.2~2.5; 1. A formula (I), methyl-2-propyl-1,3-propanediol synthesis carbonic diester compound to formula (II) shown methyl-2- propyl-1,3-propanediol and trichloromethyl chloroformate as a raw material, in an organic solvent in the organic amine catalyst -5 ~ 50 ℃ reaction was complete, the reaction was isolated as the 2-methyl - 2-propyl-1,3-propanediol diester carbonate, the 2-methyl-2-propyl-1,3-propanediol: trichloromethyl chloroformate: an organic amine catalyst ratio was 1: 0.5 to 2.5: 0.2 to 2.5;
  2. 2. 如权利要求l所述的合成方法,其特征在于所述的招:料物质的量比为2-曱基-2-丙基-1, 3-丙二醇:氯曱酸三氯曱酯:有机胺催化剂1: 0. 55~2. 0: 0.2 — 2.0。 2. The synthesis method according to claim l, wherein said trick: ratio of feed material is 2-Yue-2-propyl-1,3-propanediol: Yue-chloro-Yue acid trichloromethyl ester: organic amine catalyst 1: 0.55 - 20: 0.2 - 2.0.
  3. 3. 如权利要求1所述的合成方法,其特征在于所述的有机溶剂为下列之一或一种以上任意比例的混合物:C1〜C5的卣代烷烃、Cl-C8 的脂肪酯、C3〜C8的酉同、C2〜C8的醚。 3. The method of synthesis according to claim 1, wherein said organic solvent is a mixture of any ratio of one or more of the following: alkanes C1~C5 the wine container, Cl-C8 fatty esters, C3~ C8 is unitary with, C2~C8 ether.
  4. 4. 如权利要求1所述的合成方法,其特征在于所述的有机溶剂为苯、 曱苯、二甲苯、氯苯、硝基苯、环己烷、二硫化碳或硝基曱烷。 4. The method of synthesis according to claim 1, wherein said organic solvent is benzene, Yue benzene, xylene, chlorobenzene, nitrobenzene, cyclohexane, carbon disulfide Yue alkoxy or nitro.
  5. 5. 如权利要求3所述的合成方法,其特征在于所述的有机溶剂为下列之一或一种以上任意比例的混合物:二氯曱烷、三氯曱烷、四氯化碳、 1,1-二氯乙烷、1,2-二氯乙烷、1,1,1-三氯乙烷或1,1,2-三氯乙烷、乙酸曱酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酸异丙酯、乙酸异丁酯、乙酸戊酯、乙酸异戊酯、丙酸曱酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸戊酯、丙酮、丁酮、环己酮、乙醚、丙醚、异丙醚、丁醚、 四氬吹喃。 5. The synthesis method according to claim 3, wherein said organic solvent is a mixture of one of the following in any ratio or one or more: Yue-dichloro alkoxy, trichloromethyl Yue, carbon tetrachloride, 1, 1- dichloroethane, 1,2-dichloroethane, 1,1,1-trichloroethane or 1,1,2-trichloroethane, Yue acetate, ethyl acetate, propyl acetate, butyl acetate, isopropyl acetate, isobutyl acetate, amyl acetate, isoamyl acetate, propionate, Yue acetate, ethyl propionate, propyl propionate, butyl propionate, amyl acetate, acetone, methyl ethyl ketone, cyclohexanone, diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, tetraethylene argon blowing furans.
  6. 6. 如权利要求1所述的合成方法,其特征在于所述的有机溶剂为下列之一:乙酸甲酯、乙酸乙酯、苯、氯苯,曱苯、环己烷、环己酮、二氯曱烷、1, 2-二氯乙烷、氯仿或四氯化碳。 6. The synthesis method according to claim 1, wherein said organic solvent is one of the following: methyl acetate, ethyl acetate, benzene, chlorobenzene, Yue benzene, cyclohexane, cyclohexanone, di Yue alkyl chloride, 1,2-dichloroethane, chloroform or carbon tetrachloride.
  7. 7. 如权利要求1〜6之一所述的合成方法,其特征在于所述的有机溶剂的用量为2-曱基-2-丙基-l, 3-丙二醇质量的2~20倍。 7. The synthesis method according to one of claims 1~6, wherein an amount of said organic solvent is 2-Yue-2-propyl -l, 2 ~ 20 times the mass of 1,3-propanediol.
  8. 8. 如权利要求1所述的合成方法,其特征在于所述的有机胺催化剂为下列之一或一种以上任意比例的混合物:N,N-二甲基苯胺、吡啶、哌口定、N,N-二甲基曱酰胺、N, N-二甲基乙酰胺、三乙胺、1, 3-二曱基咪唑烷酮、N-曱基四氢吡咯、四甲基胍、曱基脲、N, N-二丁基甲酰胺或N-曱基吗啉。 8. The synthesis method according to claim 1, wherein the organic amine catalyst is a mixture of any proportion or more of the following: N, N- dimethylaniline, pyridine, piperazine port set, N , N- dimethyl amide Yue, N, N- dimethylacetamide, triethylamine, 1, 3-Yue imidazolidinone, N- Yue pyrrolidine group, tetramethylguanidine, Yue urea , N, N- dimethylformamide or N- dibutyl Yue morpholine.
  9. 9. 如权利要求1所述的合成方法,其特征在于所述的反应液分离纯化步骤为:在反应液中加入水,分离取有机层,回收溶剂,即得所述的2-曱基-2-丙基-1, 3-丙二醇磁—酸二酯- 9. The synthesis method according to claim 1, wherein said reaction liquid separation and purification steps of: adding water to the reaction mixture, the organic layer was separated, the solvent was recovered to obtain the 2-Yue group - 2-propyl-1,3-propanediol magneto - diesters -
  10. 10. 如权利要求1所述的合成方法,其特征在于所述的方法按照以下步骤进行:按照2-甲基-2-丙基-1, 3-丙二醇:有机胺催化剂的物质的量比为1: 0. 2~2. 0投料,加入有机溶剂溶解,然后緩慢滴加溶有物质的量为2-曱基-2-丙基-1, 3-丙二醇0. 55 ~ 2. 0倍的氯曱酸三氯曱酯的有机溶剂的溶液,滴加完毕后在-5〜5(TC反应4~20小时至反应完全,反应液力n水,分离耳又有机层,回收溶剂,即得所述的2-曱基-2-丙基-1, 3-丙二醇碳酸二酯;所述的有机胺催化剂为1, 3-二曱基-2-咪唑烷酮、三乙胺、N,N-二曱基曱酰胺或吡啶,所述的有机溶剂为乙酸乙酯或环己酮或氯仿。 10. The synthesis method according to claim 1, characterized in that the method is performed in the following steps: according to the 2-propyl-1,3-propanediol: the molar ratio of organic amine catalyst is 1: 0.2 ~ 20 feed, adding an organic solvent to dissolve, and then the amount of material dissolved slowly added dropwise to 2- Yue-2-propyl-1,3-propanediol 0.55 ~ 2.0 times an organic solvent solution of the acid chloride Yue Yue trichlorophenyl ester, after the addition was complete the -5~5 (TC reaction 4 to 20 hours to complete the reaction, the reaction hydraulic n water, and the organic layer was separated ear, the solvent was recovered to obtain Yue said 2-2-propyl-1,3-propanediol diester carbonate; organic amine catalyst is a 1, 3-Yue-2-imidazolidinone, triethylamine, N, N - two Yue Yue amide or pyridine group, said organic solvent is ethyl acetate or cyclohexanone or chloroform.
CN 200810122251 2008-11-06 2008-11-06 Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound CN101412705A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200810122251 CN101412705A (en) 2008-11-06 2008-11-06 Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200810122251 CN101412705A (en) 2008-11-06 2008-11-06 Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound

Publications (1)

Publication Number Publication Date
CN101412705A true true CN101412705A (en) 2009-04-22

Family

ID=40593472

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200810122251 CN101412705A (en) 2008-11-06 2008-11-06 Method for synthesizing 2-methyl-2-propyl-1,3-propanediol dimethyl carbonate compound

Country Status (1)

Country Link
CN (1) CN101412705A (en)

Similar Documents

Publication Publication Date Title
CN101139319A (en) Substituted quinoline trimer indene derivative and method for making same
Pietra et al. Question of activation by the nitro group in nucleophilic aromatic substitution
SUZUKI et al. Derivatives of 3-fluorofluorene by the Pschorr synthesis
Sam et al. Thiaindanones II. Nitration, acetylation, and mannich reactions
CN101284768A (en) Preparation method for intermediate epichlorophdrin of herbicide pretilachlor
Hamor et al. Synthesis and anticonvulsant activity of some alkyl esters of 6‐chloro‐2‐sulfamoylbenzoic acid
CN102120734A (en) Method for preparing 2-(N-alkyl)aminobenzothiazole derivatives by using active alcohol as alkylating reagent
Ellingson et al. Pyrazine chemistry. IV. Bromination of 2-amino-3-carbomethoxypyrazine
Kaplánek et al. Fast and effective reduction of nitroarenes by sodium dithionite under PTC conditions: application in solid-phase synthesis
CN102002015A (en) Air-borne preparation method for isothiazolinone and derivants thereof
CN101671299A (en) Method for synthesizing Nexavar
CN101445459A (en) Method for synthesizing 2, 4-dichloroaniline
Previtera et al. 3, 3′-Di [1, 3-thiazolidine-4-one] system. II. Anti-inflammatory and anti-histaminic properties in new substituted derivatives
Sell et al. Amino-substituted diazocines as pincer-type photochromic switches
CN101302219A (en) Fluorene derivative containing large conjugated molecule and preparation thereof
CN102093273A (en) Chemical synthesis method of sulforaphane
CN102141731A (en) Toluylene-containing meta-substituted sulfonium salt photoproduction acid agent and preparation method thereof
CN102503751A (en) Method for synthesizing alpha-brominated aromatic ketones compound
CN1424309A (en) Production of carbaminate by amine reacted with dimethyl ester carbonate
CN101445507B (en) Method for preparing praziquantel
CN104961672A (en) Synthetic method of tartrate of N-(4-fluorobenzyl)-N-(1-methylpiperidine-4-yl)-N'-(4-isobutoxybenzyl)urea
CN1394851A (en) Synthesis mothod of 1,5-naphthalene diisocyanate
CN101372451A (en) Chemical synthesis method of 2,3,4,5-phenyl tetrafluoride formyl chloride
CN104387388A (en) Novel method for synthetizing gulf-site n-heterocyclic 3,4:9,10-perylene tetracarboxylic acid diimide
CN105037061A (en) Method for synthesizing carbamic ester through alkyl boronic acid, amine and carbon dioxide

Legal Events

Date Code Title Description
C06 Publication
C10 Request of examination as to substance
C02 Deemed withdrawal of patent application after publication (patent law 2001)