Water → 2-(5-Chloropyrid-2-yl)-3-(4-ethoxycarbonylpiperazin-1-yl)carbonyloxy-isoindolin-1-one

HRID 27081노트

반응식

HRID 27081 반응식
[CH2:1]([N:3]([CH2:6][CH3:7])[CH2:4][CH3:5])C.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([N:15]2[CH:23]([O:24]C(OC3C=CC=CC=3)=O)[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]2=[O:34])=[N:13][CH:14]=1.Cl.[CH2:36]([O:38][C:39]([N:41]1CCNCC1)=[O:40])[CH3:37].[OH2:47]>C(#N)C>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([N:15]2[CH:23]([O:24][C:1]([N:3]3[CH2:6][CH2:7][N:41]([C:39]([O:38][CH2:36][CH3:37])=[O:40])[CH2:5][CH2:4]3)=[O:47])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]2=[O:34])=[N:13][CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 904381-Piperazinecarboxylic acid, ethyl ester, hydrochloride (1:1)HCID 233436562-(5-Chloropyrid-2-yl)-3-phenoxycarbonyloxy-isoindolin-1-one

생성물 1

HCID 137286492-(5-Chloropyrid-2-yl)-3-(4-ethoxycarbonylpiperazin-1-yl)carbonyloxy-isoindolin-1-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
20 °C

실험 절차

Triethylamine (3.03 g.) is added to a suspension of 2-(5-chloropyrid-2-yl)-3-phenoxycarbonyloxy-isoindolin-1-one (3.8 g.) and 1-ethoxycarbonylpiperazine hydrochloride (4.86 g.) in acetonitrile (50 cc.), and the mixture is stirred for 18 hours at a temperature of about 20° C. Water (100 cc.) is then added and the insoluble product is filtered off and washed with water (10 cc.). After drying, a product (4 g.) is obtained which, after recrystallisation from acetonitrile (30 cc.), gives 2-(5-chloropyrid-2-yl)-3-(4-ethoxycarbonylpiperazin-1-yl)carbonyloxy-isoindolin-1-one (2.8 g.) melting at 160° C.

후처리

  1. filtrationthe insoluble product is filtered off
  2. washwashed with water (10 cc.)
  3. customAfter drying
  4. customa product (4 g.) is obtained which
  5. customafter recrystallisation from acetonitrile (30 cc.)

출처 및 근거

ORD 기록
ord-5f6592c6a4384358a914cfdad510b3b6
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220646

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