CN104447327A - 甲氧基丙二酸甲乙酯的制备方法 - Google Patents

甲氧基丙二酸甲乙酯的制备方法 Download PDF

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CN104447327A
CN104447327A CN201410760574.9A CN201410760574A CN104447327A CN 104447327 A CN104447327 A CN 104447327A CN 201410760574 A CN201410760574 A CN 201410760574A CN 104447327 A CN104447327 A CN 104447327A
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mass parts
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methyl ethyl
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李涛
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CHANGSHU JINSHEN MEDICAL CHEMISTRY PRODUCTS Co Ltd
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CHANGSHU JINSHEN MEDICAL CHEMISTRY PRODUCTS Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
    • C07C67/317—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by splitting-off hydrogen or functional groups; by hydrogenolysis of functional groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
    • C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明公开了一种甲氧基丙二酸甲乙酯的制备方法，包括如下步骤：1）在反应釜中投入1.7质量份草酸二乙酯、2.4质量份甲氧基乙酸甲酯和3.3质量份固体乙醇钠，35℃保温反应3.5小时；2）再投入0.7质量份三氯乙烯，搅拌稀释；3）再投入1.3质量份水和5.2质量份35%盐酸，分出三氯乙烯；4）内温控制在85℃，水层再用三氯乙烯提取9次，回收三氯乙烯溶剂；5）在145℃，脱羰3～8小时,再减压蒸馏，得3.2质量份甲氧基丙二酸甲乙酯。本发明甲氧基丙二酸甲乙酯的制备方法，其收率高，且能大大降低能耗，适于工业化生产。

Description

甲氧基丙二酸甲乙酯的制备方法
技术领域
本发明涉及甲氧基丙二酸甲乙酯的制备方法。
背景技术
现有的甲氧基丙二酸甲乙酯的制备方法，其收率低，能耗高，不适于工业化生产。 
发明内容
本发明的目的在于提供一种甲氧基丙二酸甲乙酯的制备方法，其收率高，且能大大降低能耗，适于工业化生产。
为实现上述目的，本发明的技术方案是设计一种甲氧基丙二酸甲乙酯的制备方法，包括如下步骤：
1）在反应釜中投入1.7质量份草酸二乙酯、2.4质量份甲氧基乙酸甲酯和3.3质量份固体乙醇钠，35℃保温反应3.5小时；
2）再投入0.7质量份三氯乙烯，搅拌稀释；
3）再投入1.3质量份水和5.2质量份35%盐酸，分出三氯乙烯；
4）内温控制在85℃，水层再用三氯乙烯提取9次，回收三氯乙烯溶剂；
5）在145℃，脱羰3～8小时,再减压蒸馏，得3.2质量份甲氧基丙二酸甲乙酯。
本发明的优点和有益效果在于：提供一种甲氧基丙二酸甲乙酯的制备方法，其收率高，且能大大降低能耗，适于工业化生产。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
本发明具体实施的技术方案是：
一种甲氧基丙二酸甲乙酯的制备方法，包括如下步骤：
1）在反应釜中投入1.7质量份草酸二乙酯、2.4质量份甲氧基乙酸甲酯和3.3质量份固体乙醇钠，35℃保温反应3.5小时；
2）再投入0.7质量份三氯乙烯，搅拌稀释；
3）再投入1.3质量份水和5.2质量份35%盐酸，分出三氯乙烯；
4）内温控制在85℃，水层再用三氯乙烯提取9次，回收三氯乙烯溶剂；
5）在145℃，脱羰3～8小时,再减压蒸馏，得3.2质量份甲氧基丙二酸甲乙酯。
 
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (1)

1.甲氧基丙二酸甲乙酯的制备方法，其特征在于，包括如下步骤：
1）在反应釜中投入1.7质量份草酸二乙酯、2.4质量份甲氧基乙酸甲酯和3.3质量份固体乙醇钠，35℃保温反应3.5小时；
2）再投入0.7质量份三氯乙烯，搅拌稀释；
3）再投入1.3质量份水和5.2质量份35%盐酸，分出三氯乙烯；
4）内温控制在85℃，水层再用三氯乙烯提取9次，回收三氯乙烯溶剂；
5）在145℃，脱羰3～8小时,再减压蒸馏，得3.2质量份甲氧基丙二酸甲乙酯。
CN201410760574.9A 2014-12-13 2014-12-13 甲氧基丙二酸甲乙酯的制备方法 Pending CN104447327A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105085255A (zh) * 2015-08-12 2015-11-25 大连九信生物化工科技有限公司 一种咪唑啉酮类除草剂中间体2-烷氧基-3-氧代-丁二酸二酯的合成工艺
CN109557200A (zh) * 2018-11-23 2019-04-02 重庆康乐制药有限公司 一种采用气相色谱法监控甲氧基草乙酸甲乙酯脱羰为甲氧基丙二酸甲乙酯反应终点的方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304094A (zh) * 2011-09-23 2012-01-04 常熟市南湖实业化工有限公司 一种周效磺胺及其中间体的制备方法
CN102304095A (zh) * 2011-09-23 2012-01-04 常熟市南湖实业化工有限公司 一种周效磺胺的制备方法
CN103864700A (zh) * 2014-03-10 2014-06-18 常熟市金申医化制品有限责任公司 5-甲氧基-4,6-二羟嘧啶二钠的制备方法
CN103910684A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 4,6-二羟基-5-甲氧基嘧啶钠的制备方法
CN103910630A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 甲氧基丙二酸甲乙酯的制备方法
CN103910629A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 一种平稳制备甲氧基丙二酸甲乙酯的方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304094A (zh) * 2011-09-23 2012-01-04 常熟市南湖实业化工有限公司 一种周效磺胺及其中间体的制备方法
CN102304095A (zh) * 2011-09-23 2012-01-04 常熟市南湖实业化工有限公司 一种周效磺胺的制备方法
CN103864700A (zh) * 2014-03-10 2014-06-18 常熟市金申医化制品有限责任公司 5-甲氧基-4,6-二羟嘧啶二钠的制备方法
CN103910684A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 4,6-二羟基-5-甲氧基嘧啶钠的制备方法
CN103910630A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 甲氧基丙二酸甲乙酯的制备方法
CN103910629A (zh) * 2014-03-10 2014-07-09 常熟市南湖实业化工有限公司 一种平稳制备甲氧基丙二酸甲乙酯的方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105085255A (zh) * 2015-08-12 2015-11-25 大连九信生物化工科技有限公司 一种咪唑啉酮类除草剂中间体2-烷氧基-3-氧代-丁二酸二酯的合成工艺
CN105085255B (zh) * 2015-08-12 2018-03-09 内蒙古佳瑞米精细化工有限公司 一种咪唑啉酮类除草剂中间体2‑烷氧基‑3‑氧代‑丁二酸二酯的合成工艺
CN109557200A (zh) * 2018-11-23 2019-04-02 重庆康乐制药有限公司 一种采用气相色谱法监控甲氧基草乙酸甲乙酯脱羰为甲氧基丙二酸甲乙酯反应终点的方法

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Application publication date: 20150325