CN1772742A - 高纯度2,6-二氯喹喔啉的制备方法 - Google Patents

高纯度2,6-二氯喹喔啉的制备方法 Download PDF

Info

Publication number
CN1772742A
CN1772742A CN 200510095624 CN200510095624A CN1772742A CN 1772742 A CN1772742 A CN 1772742A CN 200510095624 CN200510095624 CN 200510095624 CN 200510095624 A CN200510095624 A CN 200510095624A CN 1772742 A CN1772742 A CN 1772742A
Authority
CN
China
Prior art keywords
dichloro
organic solvent
preparation
high purity
quinozaline
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
CN 200510095624
Other languages
English (en)
Other versions
CN100345831C (zh
Inventor
吴永虎
赵邦斌
何普泉
苏朝辉
陈克付
孙澎
丁云好
陆广美
Original Assignee
吴永虎
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
Application filed by 吴永虎 filed Critical 吴永虎
Priority to CNB2005100956247A priority Critical patent/CN100345831C/zh
Publication of CN1772742A publication Critical patent/CN1772742A/zh
Application granted granted Critical
Publication of CN100345831C publication Critical patent/CN100345831C/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)

Abstract

高纯度2,6-二氯喹喔啉的制备方法,属精细化工产品制备技术领域。其所要解决的技术问题是:提供一种无须多次提纯即能够在农药尤其是医药上普遍应用的高纯度2,6-二氯喹喔啉的制备方法。其技术要点是:将反应物6氯-2-羟基-喹喔啉与氯化剂按1∶2.5~3.5的摩尔比及催化剂加入到有机溶剂体系中,搅拌后升温至回流状况下反应;反应完毕后脱去大部分的溶剂,然后再加入溶剂及水,用液碱调节pH值至6~7之间;加入脱色剂,过滤至蒸馏釜,脱去有机溶剂后即得2,6-二氯喹喔啉。其含量大于99%以上,能广泛应用于农药和医药业,大大拓宽了其使用范围。且其制备方法极其简单,工艺过程简单可控,既无需增加任何设备投资,也不增加劳动量。

Description

高纯度2,6-二氯喹喔啉的制备方法
技术领域:本发明属于精细化工产品制备技术,特别是一种高纯度2,6-二氯喹喔啉的制备方法。
背景技术:目前,工业上合成的2,6-二氯喹喔啉一次出料的含量最高仅为94%左右,作为中间体,其含量不能完全满足后续合成的要求,使其在农药尤其是在医药上的应用受到较大的限制。若需进一步提高含量,则需多次提纯,但如此一来,既大幅度地降低了收率,增加了生产成本,又增加了生产劳动量。
发明内容:本发明所要解决的技术问题是:提供一种无须多次提纯即能够在农药尤其是在医药上普遍应用的高纯度2,6-二氯喹喔啉的制备方法,且该制备方法简单可控。其技术方案是:一种高纯度2、6-二氯喹喔啉的制备方法,其技术特征在于:
(1)、将反应物6氯-2-羟基-喹喔啉与氯化剂按1∶2.5~3.5的摩尔比及催化剂加入到有机溶剂体系中,搅拌后升温至回流状况下反应5~10小时;
(2)、反应完毕后脱去大部分的溶剂,然后再加入溶剂及水,用液碱调节PH值至6~7之间;
(3)、加入脱色剂,过滤至蒸馏釜,脱去有机溶剂后即得2,6-二氯喹喔啉。
上述的氯化剂为氯化亚砜或三氯氧磷。
上述的催化剂为DMF或DMA。
上述的有机溶剂为甲苯。
其技术效果为:
1、采用本发明的制备方法所生产出的2,6-二氯喹喔啉,其含量大于99%以上,能广泛应用于农药和医药业,大大拓宽了其使用范围。
2、本发明的制备方法极其简单、可靠,工艺过程简单可控,设备投资少,劳动强度低。
具体实施方式:
将110ml甲苯、8.4克6-氯-2-羟基喹喔啉、1.6克DMF、15克氯化亚砜投入到装有搅拌、冷凝器及温度计的250ml反应瓶中,投料完毕,搅拌升温至回流状态,保持温度在96~108℃之间,保温反应6小时,反应完毕后脱出有机溶剂及部分未反应完全的氯化剂(约85ml的母液,母液可套用)。然后在微负压下向体系中加入80ml的甲苯和40ml的水,破坏剩余的少量SOCl2(克氯化亚砜),滴加液碱调节PH值至6-7之间,加入1g活性炭脱色后经板框过滤至蒸馏釜,分去下层少量絮状物后用水共沸脱出约95%左右的甲苯后降温板框出料,水洗、吹压气,干燥后即得8.5g的2,6-二氯喹喔啉,GC分析含量大于99.5%,收率大于96%。

Claims (4)

1、一种高纯度2、6-二氯喹喔啉的制备方法,其技术特征在于:
(1)、将反应物6氯-2-羟基-喹喔啉与氯化剂按1∶2.5~3.5的摩尔比及催化剂加入到有机溶剂体系中,搅拌后升温至回流状况下反应5~10小时;
(2)、反应完毕后脱去大部分的溶剂,然后再加入溶剂及水,用液碱调节PH值至6~7之间;
(3)、加入脱色剂,过滤至蒸馏釜,脱去有机溶剂后即得2,6-二氯喹喔啉。
2、根据权利要求1所述的一种制备方法,其特征置于:所述的氯化剂为氯化亚砜或三氯氧磷。
3、根据权利要求1所述的一种制备方法,其特征置于:所述的催化剂为DMF或DMA。
4、根据权利要求1所述的一种制备方法,其特征置于:所述的有机溶剂为甲苯。
CNB2005100956247A 2005-11-10 2005-11-10 高纯度2,6-二氯喹喔啉的制备方法 Active CN100345831C (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2005100956247A CN100345831C (zh) 2005-11-10 2005-11-10 高纯度2,6-二氯喹喔啉的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2005100956247A CN100345831C (zh) 2005-11-10 2005-11-10 高纯度2,6-二氯喹喔啉的制备方法

Publications (2)

Publication Number Publication Date
CN1772742A true CN1772742A (zh) 2006-05-17
CN100345831C CN100345831C (zh) 2007-10-31

Family

ID=36759903

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2005100956247A Active CN100345831C (zh) 2005-11-10 2005-11-10 高纯度2,6-二氯喹喔啉的制备方法

Country Status (1)

Country Link
CN (1) CN100345831C (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914069A (zh) * 2010-07-29 2010-12-15 安徽丰乐农化有限责任公司 6-氯-2-羟基喹喔啉的氯化新工艺

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EG11837A (en) * 1974-09-19 1977-12-31 Lilly Co Eli Novel 1-(substituted benzoyl)-3-(substituted pyrazinyl ureas used as insecticides
DE2724624C2 (de) * 1977-06-01 1985-07-25 Carl Schenck Ag, 6100 Darmstadt Verfahren zum Eindrehen eines mit Unwucht behafteten Rotationskörpers
US4636562A (en) * 1982-05-07 1987-01-13 E. I. Du Pont De Nemours And Company Process for preparing 6-halo-2-chloroquinoxaline
EP0113831A3 (de) * 1982-12-17 1984-11-07 F. HOFFMANN-LA ROCHE & CO. Aktiengesellschaft Carbaminsäureester, Verfahren zu deren Herstellung und deren Verwendung
DE3925969A1 (de) * 1989-08-05 1991-02-07 Hoechst Ag Verfahren zur herstellung von 2,6-dichlorchinoxalin
US5529999A (en) * 1994-03-04 1996-06-25 Eli Lilly And Company Antitumor compositions and methods of treatment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914069A (zh) * 2010-07-29 2010-12-15 安徽丰乐农化有限责任公司 6-氯-2-羟基喹喔啉的氯化新工艺

Also Published As

Publication number Publication date
CN100345831C (zh) 2007-10-31

Similar Documents

Publication Publication Date Title
CN1834092B (zh) 盐酸普拉克索的制备方法
CN105254575B (zh) 一种磺胺嘧啶的合成方法
CN105924428A (zh) 一种合成吡虫啉的方法
CN104130198B (zh) 2-氨基-4,6-二甲氧基嘧啶及其制备方法
CN104961710A (zh) 一种呋虫胺的合成方法
CN108440409B (zh) 一种瑞巴匹特的绿色高效制备方法
CN102417472B (zh) 一种氟苯尼考的制备方法
CN100345831C (zh) 高纯度2,6-二氯喹喔啉的制备方法
CN110452181B (zh) 2-甲基-4-氨基-5-甲酰胺甲基嘧啶的合成方法
CN102838481A (zh) 3,5-二氯苯甲酰氯的合成
CN101560132B (zh) 手性氨基酸或其衍生物的消旋方法
CN104496936B (zh) 一种盐酸普拉克索的制备方法
JP5000645B2 (ja) 3,4−ジクロロイソチアゾールカルボン酸の調製方法
CN111470963A (zh) 一种制备苯氧乙酸及制备2,4-二氯苯氧乙酸的方法
CN102391170B (zh) 一种n,n-二烯丙基-5-甲氧基色胺盐酸盐的制备方法
CN111269144A (zh) 一种氨基苯甲腈的制备方法
CN1067993C (zh) 乙二醛一步合成尿囊素的方法
CN110938036A (zh) 一种4-碘-1h-咪唑的制备方法
CN105669539B (zh) 一种2-氨基-3-氟吡啶的制备工艺
CN101054398B (zh) 2-脱氧-5-碘代-β-尿苷的合成方法
CN115677523B (zh) 一种2,6-二氟苯甲酰胺的制备方法
CN101054366B (zh) 1-甲基海因的合成方法
CN110483334B (zh) 一种对羟基苯甲腈的高效合成方法
CN106866522A (zh) 一种异烟肼的合成方法
CN109320472B (zh) 一种3,4-二氯5-氰基异噻唑的制备方法

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20090220

Address after: No. 4, Pioneer Road, Shushan Economic Development Zone, Anhui, Hefei

Patentee after: Anhui Fengle Agrochemical Co., Ltd.

Address before: Anhui city of Hefei Province Agricultural Company fan wa Road No. 8

Patentee before: Wu Yonghu

ASS Succession or assignment of patent right

Owner name: ANHUI FENGLE AGRICULTURAL CO., LTD.

Free format text: FORMER OWNER: WU YONGHU

Effective date: 20090220

C56 Change in the name or address of the patentee
CP02 Change in the address of a patent holder

Address after: 231602 Hefei circular economy demonstration garden, Feidong County, Anhui Province

Patentee after: Anhui Fengle Agrochemical Co., Ltd.

Address before: 230031 No. 4, Pioneer Road, Shushan Economic Development Zone, Anhui, Hefei

Patentee before: Anhui Fengle Agrochemical Co., Ltd.

PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high-purity 2-methyl-4-chloro phenoxyacetic acid

Effective date of registration: 20160809

Granted publication date: 20071031

Pledgee: Bank of Hangzhou, Limited by Share Ltd, Feidong branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2016340000042

PLDC Enforcement, change and cancellation of contracts on pledge of patent right or utility model
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20170803

Granted publication date: 20071031

Pledgee: Bank of Hangzhou, Limited by Share Ltd, Feidong branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2016340000042

PC01 Cancellation of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high-purity 2-methyl-4-chloro phenoxyacetic acid

Effective date of registration: 20170814

Granted publication date: 20071031

Pledgee: Bank of Hangzhou, Limited by Share Ltd, Feidong branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2017340000151

PE01 Entry into force of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20170818

Granted publication date: 20071031

Pledgee: Bank of Hangzhou, Limited by Share Ltd, Feidong branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2017340000151

PC01 Cancellation of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Process for preparing high-purity 2-methyl-4-chloro phenoxyacetic acid

Effective date of registration: 20170828

Granted publication date: 20071031

Pledgee: Industrial Bank Limited by Share Ltd Hefei branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2017340000180

PE01 Entry into force of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20190129

Granted publication date: 20071031

Pledgee: Industrial Bank Limited by Share Ltd Hefei branch

Pledgor: Anhui Fengle Agrochemical Co., Ltd.

Registration number: 2017340000180

PC01 Cancellation of the registration of the contract for pledge of patent right