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

HRID 27081ノート

反応式

HRID 27081 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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.)

出典と根拠

ORDレコード
ord-5f6592c6a4384358a914cfdad510b3b6
出典データセット
uspto-grants-1980_09
特許番号
US04220646

反応ノート

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