1-Chloroethyl chloroformate → HCID 178485767、化合物

HRID 24778

反応式

HRID 24778 の反応式
C([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]([N:17]([C:19]2[CH:24]=[CH:23][C:22]([NH:25]/[C:26](=[C:33]3\[C:34](=[O:42])[NH:35][C:36]4[C:41]\3=[CH:40][CH:39]=[CH:38][CH:37]=4)/[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:21][CH:20]=2)[CH3:18])=[O:16])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:43]C(OC(Cl)C)=O>ClCCl>[ClH:43].[ClH:43].[N:11]1([CH2:14][C:15]([N:17]([C:19]2[CH:24]=[CH:23][C:22]([NH:25]/[C:26](=[C:33]3\[C:34](=[O:42])[NH:35][C:36]4[C:41]\3=[CH:40][CH:39]=[CH:38][CH:37]=4)/[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:21][CH:20]=2)[CH3:18])=[O:16])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 178485769HCID 178485769、化合物

生成物 1

HCID 178485767HCID 178485767、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

390 mg (0.7 mmol) of (Z)-3-{1-[4-(N—(N-benzylpiperazinomethylcarbonyl)-N-methylamino)-phenylamino]-1-phenyl-methylidene}-2-indolinone are dissolved in 20 ml of dichloromethane and after the addition of 0.2 g (1.4 mmol) of 1-chloroethyl chloroformate heated for 30 minutes at ambient temperature and refluxed for 60 minutes. The solvent is concentrated by evaporation, the residue is combined with 10 ml of methanol and refluxed for 90 minutes. After 18 hours stirring at ambient temperature, the product is suction filtered, washed with methanol and dried.

後処理

  1. temperaturerefluxed for 60 minutes
  2. concentrationThe solvent is concentrated by evaporation
  3. temperaturerefluxed for 90 minutes
  4. filtrationfiltered
  5. washwashed with methanol
  6. customdried

出典と根拠

ORDレコード
ord-1e02debe0c2c40d8bd1bb285536265c9
出典データセット
uspto-grants-2005_02
特許番号
US06855710B2

関連ノート

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