CN114072389A - 一种5-氟尿嘧啶的组合物及其精制方法 - Google Patents

一种5-氟尿嘧啶的组合物及其精制方法 Download PDF

Info

Publication number
CN114072389A
CN114072389A CN202080046813.8A CN202080046813A CN114072389A CN 114072389 A CN114072389 A CN 114072389A CN 202080046813 A CN202080046813 A CN 202080046813A CN 114072389 A CN114072389 A CN 114072389A
Authority
CN
China
Prior art keywords
fluorouracil
less
impurities
water
refining
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
CN202080046813.8A
Other languages
English (en)
Other versions
CN114072389B (zh
Inventor
陈小林
高鹏飞
杨易可
梁屹
占娅锋
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.)
Shanghai Xudong Haipu Pharmaceutical Co ltd
Original Assignee
Shanghai Xudong Haipu 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 Shanghai Xudong Haipu Pharmaceutical Co ltd filed Critical Shanghai Xudong Haipu Pharmaceutical Co ltd
Publication of CN114072389A publication Critical patent/CN114072389A/zh
Application granted granted Critical
Publication of CN114072389B publication Critical patent/CN114072389B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
    • C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
    • C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
    • C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
    • C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
    • C07D239/52—Two oxygen atoms
    • C07D239/54—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals
    • C07D239/545—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals with other hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
    • C07D239/553—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals with other hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms with halogen atoms or nitro radicals directly attached to ring carbon atoms, e.g. fluorouracil

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

本发明公开了一种5‑氟尿嘧啶的精制方法，包括以下步骤，将5‑氟尿嘧啶溶解在有机溶剂优选DMSO中，加热搅拌至溶解；滤液自然冷却至析出晶体；过滤，滤饼用极性溶剂洗涤以及抽干减压干燥的过程。采用这种新型的精制方法，可将5‑氟尿嘧啶中杂质的含量降低至0.01％以下，产品纯度99.98％以上，精制收率高于70％。另外本发明的精制方法工艺过程简单、操作方便、生产成本低廉、产物纯度高、工艺稳定、适合工业化生产。

Description

PCT国内申请，说明书已公开。

Claims (10)

  1. PCT国内申请，权利要求书已公开。
CN202080046813.8A 2019-08-05 2020-01-10 一种5-氟尿嘧啶的组合物及其精制方法 Active CN114072389B (zh)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CN201910716013.1A CN110372610B (zh) 2019-08-05 2019-08-05 一种5-氟尿嘧啶的组合物及其精制方法
CN2019107160131 2019-08-05
PCT/CN2020/071350 WO2021022788A1 (zh) 2019-08-05 2020-01-10 一种5-氟尿嘧啶的组合物及其精制方法

Publications (2)

Publication Number Publication Date
CN114072389A true CN114072389A (zh) 2022-02-18
CN114072389B CN114072389B (zh) 2023-09-08

Family

ID=68258134

Family Applications (2)

Application Number Title Priority Date Filing Date
CN201910716013.1A Active CN110372610B (zh) 2019-08-05 2019-08-05 一种5-氟尿嘧啶的组合物及其精制方法
CN202080046813.8A Active CN114072389B (zh) 2019-08-05 2020-01-10 一种5-氟尿嘧啶的组合物及其精制方法

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN201910716013.1A Active CN110372610B (zh) 2019-08-05 2019-08-05 一种5-氟尿嘧啶的组合物及其精制方法

Country Status (3)

Country Link
US (1) US11866413B2 (zh)
CN (2) CN110372610B (zh)
WO (1) WO2021022788A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925639A (zh) * 2023-01-31 2023-04-07 上海旭东海普南通药业有限公司 一种抗肿瘤氟尿嘧啶及其制备工艺

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110372610B (zh) * 2019-08-05 2020-05-22 上海旭东海普药业有限公司 一种5-氟尿嘧啶的组合物及其精制方法
CN113121453A (zh) * 2019-12-31 2021-07-16 精华制药集团南通有限公司 一种制备5-氟尿嘧啶的绿色制备工艺
CN114210238A (zh) * 2021-12-02 2022-03-22 上海旭东海普南通药业有限公司 一种氟尿嘧啶精制方法及装置
CN114436973A (zh) * 2022-03-11 2022-05-06 国药一心制药有限公司 一种氟尿嘧啶新晶型及其制备方法和应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005089511A2 (en) * 2004-03-19 2005-09-29 Transform Pharmaceuticals, Inc. Novel pharmaceutical forms, and methods of making and using the same
CN104447576A (zh) * 2014-11-21 2015-03-25 山东金城医药化工股份有限公司 5-氟尿嘧啶的制备方法
CN107963994A (zh) * 2018-01-22 2018-04-27 精华制药集团南通有限公司 一种制备5-氟尿嘧啶的绿色方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110372610B (zh) * 2019-08-05 2020-05-22 上海旭东海普药业有限公司 一种5-氟尿嘧啶的组合物及其精制方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005089511A2 (en) * 2004-03-19 2005-09-29 Transform Pharmaceuticals, Inc. Novel pharmaceutical forms, and methods of making and using the same
CN104447576A (zh) * 2014-11-21 2015-03-25 山东金城医药化工股份有限公司 5-氟尿嘧啶的制备方法
CN107963994A (zh) * 2018-01-22 2018-04-27 精华制药集团南通有限公司 一种制备5-氟尿嘧啶的绿色方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
M.P.CAVA 等: "A convenient synthesis of 5-Fluorouracil", 《J.ORG.CHEM》, vol. 37, no. 2, pages 329 - 330 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925639A (zh) * 2023-01-31 2023-04-07 上海旭东海普南通药业有限公司 一种抗肿瘤氟尿嘧啶及其制备工艺

Also Published As

Publication number Publication date
CN110372610B (zh) 2020-05-22
CN114072389B (zh) 2023-09-08
CN110372610A (zh) 2019-10-25
US20220348548A1 (en) 2022-11-03
US11866413B2 (en) 2024-01-09
WO2021022788A1 (zh) 2021-02-11

Similar Documents

Publication Publication Date Title
CN110372610B (zh) 一种5-氟尿嘧啶的组合物及其精制方法
US20060199954A1 (en) Purification of rapamycin
CN108997355B (zh) 一种枸橼酸托法替尼化合物的精制方法
AU2013330603B2 (en) Monohydrate crystal of fimasartan potassium salt, method for preparing same, and pharmacological composition comprising same
WO2020010643A1 (zh) 一种缬沙坦的合成方法
US3463850A (en) Arabinofuranosyl 2-thiopyrimidines and pharmaceutical compositions thereof
JP6980779B2 (ja) 肝臓送達に基づく抗ウイルス性プロドラッグであるヌクレオシド環状リン酸エステル化合物およびその使用
EP2646431B1 (en) A process for the preparation of pazopanib using novel intermediate
EP2956439B1 (en) Process for preparing atazanavir sulphate
US7183272B2 (en) Crystal forms of oxcarbazepine and processes for their preparation
TWI668222B (zh) 5型磷酸二酯酶抑制劑的甲磺酸鹽多晶物及其製備方法和應用
AU764594B2 (en) Crystal forms of 3-(2,4-dichlorobenzyl)-2-methyl-N- (pentylsulfonyl)-3H-benzimidazole-5-carboxamide
CN115925639A (zh) 一种抗肿瘤氟尿嘧啶及其制备工艺
CN111689958B (zh) 磷酸二酯酶抑制剂的晶型、其制备方法及其用途
US10174001B2 (en) Crystals of 5-cyclopropyl-2-((1-(3-fluorobenzyl)-1H-indol-5-yl)amino)nicotinic acid
CN104163769A (zh) 一种氯化丙酰左卡尼汀的制备方法
CN108383859B (zh) 咪唑并苯并噻唑醚类化合物及其可药用盐制备方法和应用
CN109970736A (zh) 一种他达拉非结晶方法
CN110903291B (zh) 一种杂芳基并[4,3-c]嘧啶-5-胺类衍生物的盐、盐的晶型及制备方法
JP3068175B2 (ja) イソチアゾロ〔５，４―ｂ〕ピリジン誘導体
CN108863946B (zh) 一种地巴唑杂质对照品的制备方法
CN106957311B (zh) 雷替曲塞的溶剂化物及其制备方法
JP3002507B2 (ja) 四環式化合物
CN113861106A (zh) 一种高纯度药用吉美嘧啶的生产工艺
CN114436973A (zh) 一种氟尿嘧啶新晶型及其制备方法和应用

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