Piperazine → 2-(7-Chloro-1,8-naphthyridin-2-yl)-3-(piperazin-1-yl)carbonyloxy-isoindolin-1-one

HRID 259652

反応式

HRID 259652 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[N:17]=[C:16]2[C:11]([CH:12]=[CH:13][C:14]([N:18]3[CH:26]([O:27][C:28](OC4C=CC=CC=4)=[O:29])[C:25]4[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=4)[C:19]3=[O:37])=[N:15]2)=[CH:10][CH:9]=1.C(OC(C)C)(C)C>C(#N)C>[Cl:7][C:8]1[N:17]=[C:16]2[C:11]([CH:12]=[CH:13][C:14]([N:18]3[CH:26]([O:27][C:28]([N:1]4[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]4)=[O:29])[C:25]4[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=4)[C:19]3=[O:37])=[N:15]2)=[CH:10][CH:9]=1

参加物

5

反応物 3

HCID 4837PiperazineHCID 7914Diisopropyl EtherHCID 233436372-(7-Chloro-1,8-naphthyridin-2-yl)-3-phenoxycarbonyloxy-1-isoindolinone

生成物 1

HCID 233436392-(7-Chloro-1,8-naphthyridin-2-yl)-3-(piperazin-1-yl)carbonyloxy-isoindolin-1-one収率 47%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Anhydrous piperazine (5.15 g.) is added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-3-phenoxycarbonyloxy-isoindolin-1-one (5.2 g.) in acetonitrile (32 cc.). The reaction mixture is stirred for 1 hour at a temperature of about 20° C. and diisopropyl ether (150 cc.) is then added. The insoluble product is filtered off and washed with a mixture (20 cc.) of acetonitrile and diisopropyl ether (50--50 by volume) and then with diisopropyl ether (50 cc.). After recrystallisation of the product thus obtained from a mixture (160 cc.) of acetonitrile and methanol (90- 10 by volume), 2-(7-chloro-1,8-naphthyridin-2-yl)-3-(piperazin-1-yl)carbonyloxy-isoindolin-1-one (2.4 g.), melting with decomposition at 245° C., is obtained.

後処理

  1. additionis then added
  2. filtrationThe insoluble product is filtered off
  3. washwashed with a mixture (20 cc.) of acetonitrile and diisopropyl ether (50--50 by volume)
  4. customAfter recrystallisation of the product

出典と根拠

ORDレコード
ord-9b564f632d694613a2f8f05d8754c4f4
出典データセット
uspto-grants-1977_07
特許番号
US04038391

関連ノート

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