CN107074750A - 一种拆分西酞普兰中间体5‑氰二醇的方法 - Google Patents

一种拆分西酞普兰中间体5‑氰二醇的方法 Download PDF

Info

Publication number
CN107074750A
CN107074750A CN201480081785.8A CN201480081785A CN107074750A CN 107074750 A CN107074750 A CN 107074750A CN 201480081785 A CN201480081785 A CN 201480081785A CN 107074750 A CN107074750 A CN 107074750A
Authority
CN
China
Prior art keywords
ether
solvent
ethylene glycol
water
resolving
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
CN201480081785.8A
Other languages
English (en)
Other versions
CN107074750B (zh
Inventor
梁尊俊
胡斯琪
彭才华
黄文峰
芦启锋
涂国良
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Huahai Pharmaceutical Co Ltd
Original Assignee
Zhejiang Huahai Pharmaceutical Co Ltd
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 Zhejiang Huahai Pharmaceutical Co Ltd filed Critical Zhejiang Huahai Pharmaceutical Co Ltd
Publication of CN107074750A publication Critical patent/CN107074750A/zh
Application granted granted Critical
Publication of CN107074750B publication Critical patent/CN107074750B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C255/00Carboxylic acid nitriles
    • C07C255/49Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C255/50Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton to carbon atoms of non-condensed six-membered aromatic rings
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C255/00Carboxylic acid nitriles
    • C07C255/49Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C255/58Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing cyano groups and singly-bound nitrogen atoms, not being further bound to other hetero atoms, bound to the carbon skeleton
    • C07C255/59Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing cyano groups and singly-bound nitrogen atoms, not being further bound to other hetero atoms, bound to the carbon skeleton the carbon skeleton being further substituted by singly-bound oxygen atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C69/00Esters of carboxylic acids; Esters of carbonic or haloformic acids
    • C07C69/76Esters of carboxylic acids having a carboxyl group bound to a carbon atom of a six-membered aromatic ring
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C69/00Esters of carboxylic acids; Esters of carbonic or haloformic acids
    • C07C69/76Esters of carboxylic acids having a carboxyl group bound to a carbon atom of a six-membered aromatic ring
    • C07C69/78Benzoic acid esters
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs

Landscapes

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

Abstract

提供了一种拆分式4‑[4‑二甲氨基‑1‑(4‑氟苯基)‑1‑羟基丁基]‑3‑羟甲基苯腈为其对映异构体的方法,包括以下步骤:在拆分溶剂中结晶出(S)‑4‑[4‑二甲氨基‑1‑(4‑氟苯基)‑1‑羟基丁基]‑3‑羟甲基苯腈与拆分剂D‑(+)二对甲苯甲酰酒石酸形成的盐;其特征在于所述的拆分溶剂为醚类溶剂。还提供了拆分中间体新晶型。

Description

PCT国内申请,说明书已公开。

Claims (8)

  1. PCT国内申请,权利要求书已公开。
CN201480081785.8A 2014-11-14 2014-11-14 一种拆分西酞普兰中间体5-氰二醇的方法 Active CN107074750B (zh)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2014/091139 WO2016074225A1 (zh) 2014-11-14 2014-11-14 一种拆分西酞普兰中间体5-氰二醇的方法

Publications (2)

Publication Number Publication Date
CN107074750A true CN107074750A (zh) 2017-08-18
CN107074750B CN107074750B (zh) 2022-03-25

Family

ID=55953616

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201480081785.8A Active CN107074750B (zh) 2014-11-14 2014-11-14 一种拆分西酞普兰中间体5-氰二醇的方法

Country Status (5)

Country Link
US (2) US10287240B2 (zh)
EP (1) EP3219702B1 (zh)
CN (1) CN107074750B (zh)
ES (1) ES2881105T3 (zh)
WO (1) WO2016074225A1 (zh)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006106531A1 (en) * 2005-04-04 2006-10-12 Jubilant Organosys Ltd Process for the preparation of escitalopram or its acid addition salts
WO2008059514A2 (en) * 2006-07-31 2008-05-22 Cadila Healthcare Limited Process for preparing escitalopram
CN101460448A (zh) * 2006-01-23 2009-06-17 桑多斯股份公司 羰基不对称烷基化
US20110092719A1 (en) * 2008-06-16 2011-04-21 Shodhana Laboratories Limited Preparation of Escitalopram, Its Salts and Intermediates

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8814057D0 (en) * 1988-06-14 1988-07-20 Lundbeck & Co As H New enantiomers & their isolation
WO2007012954A1 (en) * 2005-07-27 2007-02-01 Aurobindo Pharma Limited An improved process for the preparation of escitalopram
FI121570B (fi) 2007-09-11 2011-01-14 Lundbeck & Co As H Menetelmä essitalopraamin valmistamiseksi
JP5256749B2 (ja) * 2008-01-23 2013-08-07 住友化学株式会社 乳剤組成物
CN101265215B (zh) * 2008-04-18 2011-03-16 浙江奥托康制药集团股份有限公司 一种右旋西酞普兰中间体s-型二醇的制备方法
CN102190600B (zh) * 2010-03-13 2015-04-15 浙江华海药业股份有限公司 一种右旋西酞普兰中间体s-型二醇的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006106531A1 (en) * 2005-04-04 2006-10-12 Jubilant Organosys Ltd Process for the preparation of escitalopram or its acid addition salts
CN101460448A (zh) * 2006-01-23 2009-06-17 桑多斯股份公司 羰基不对称烷基化
WO2008059514A2 (en) * 2006-07-31 2008-05-22 Cadila Healthcare Limited Process for preparing escitalopram
US20110092719A1 (en) * 2008-06-16 2011-04-21 Shodhana Laboratories Limited Preparation of Escitalopram, Its Salts and Intermediates

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
姚忠科,阚丽娟: "草酸依地普仑的合成", 《中国新药杂志》 *
金俊华 等: "草酸依地普仑的合成", 《广州化工》 *

Also Published As

Publication number Publication date
US10287240B2 (en) 2019-05-14
US10508076B2 (en) 2019-12-17
WO2016074225A1 (zh) 2016-05-19
US20190185418A1 (en) 2019-06-20
US20170240505A1 (en) 2017-08-24
EP3219702A1 (en) 2017-09-20
CN107074750B (zh) 2022-03-25
ES2881105T3 (es) 2021-11-26
EP3219702A4 (en) 2018-05-30
EP3219702B1 (en) 2021-05-05

Similar Documents

Publication Publication Date Title
JP7085641B2 (ja) アルコラート塩基の存在下でのニコチン酸エチルとn-ビニルピロリドンとの反応によるラセミ体ニコチンの調製方法
JP6378844B2 (ja) 第6結晶形ソホスブビルの調製方法
KR20130129180A (ko) 아미노벤조일벤조푸란 유도체의 제조 방법
KR102565407B1 (ko) 극성 비양자성 용매를 이용한 n-[4-(1-아미노에틸)-페닐]-술폰아미드 유도체의 카이랄 분할 방법
CN104003863A (zh) 一种安息香的绿色合成方法
CN105503638A (zh) 沙库比曲二环己胺盐、晶型及其制备方法
CN106928149B (zh) 一种奥拉帕尼的制备方法
JP6137185B2 (ja) (r)−1,1,3−トリメチル−4−アミノインダンの製造方法
EP2178826A1 (en) Process and intermediates for the synthesis of 1,2-substituted 3,4-dioxo-1-cyclobutene compounds
KR20160125115A (ko) 3-히드록시테트라하이드로퓨란의 제조방법
CN106065005B (zh) R-(+)-2-[4-(羟基苯氧基)]丙酸酯的制备方法
CN101838188A (zh) 甲基或乙基香兰素的精制方法
CN107074750B (zh) 一种拆分西酞普兰中间体5-氰二醇的方法
WO2016146049A1 (zh) 一种咪达唑仑的工业制造方法
WO2016146048A1 (zh) 一种咪达唑仑衍生物的工业制造方法
CN104703967B (zh) 氟伏沙明游离碱的精制方法及利用其的高纯度马来酸氟伏沙明的制备方法
EP3452446B1 (de) Verfahren zur herstellung von cis-alkoxysubstituierten spirocyclischen 1-h-pyrrolidin-2,4-dion- derivaten
CN104876812B (zh) 制备盐酸舍曲林中间体及杂质的方法
CN102190600A (zh) 一种右旋西酞普兰中间体s-型二醇的制备方法
CN101514163B (zh) 光学纯西布曲明及其衍生盐的制备工艺
SU602112A3 (ru) Способ получени аминов, или их солей, рацематов или оптическиактивных антиподов
KR102556971B1 (ko) 데커시놀((+)-Decursinol)의 신규한 제조방법
CN105461656A (zh) 一种制备沃替西汀的新工艺
CN102757414B (zh) 艾司西酞普兰草酸盐的制备方法
CN109369367A (zh) 一种木质素制备4-(3-羟基苯基)-4-氧代丁酸的方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant