Triethylamine → 4-(6,7-Dimethoxy-4-quinazolinyl)-1-piperazinethiocarboxylic acid chloride

HRID 353158

反応式

HRID 353158 の反応式
[C:1]([Cl:4])(Cl)=[S:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][CH3:18])[N:13]=[CH:12][N:11]=[C:10]2[N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(N(CC)CC)C>ClCCl>[CH3:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][CH3:18])[N:13]=[CH:12][N:11]=[C:10]2[N:19]1[CH2:20][CH2:21][N:22]([C:1]([Cl:4])=[S:2])[CH2:23][CH2:24]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 27584846,7-Dimethoxy-4-piperazin-1-yl-quinazoline

生成物 1

HCID 109262444-(6,7-Dimethoxy-4-quinazolinyl)-1-piperazinethiocarboxylic acid chloride収率 52%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 3.06 ml (40.1 mmol) of thiophosgene in 100 ml of dichloromethane were slowly added a solution of 10 g (36.5 mmol) of 6,7-dimethoxy-4-(1-piperazinyl)quinazoline obtained by the method described in South African Patent No. 67 06512 (1968) in 100 ml of dichloromethane and 12.4 ml (89.1 mmol) of triethylamine under ice-cooling. The resulting mixture was stirred at the same temperature in an atmosphere of argon for 2 hours. After the solvent was evaporated, the residue was purified by silica gel chromatography to give 6.65 g (52%) of the desired compound.

後処理

  1. customobtained by the method
  2. customAfter the solvent was evaporated
  3. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-2443a5210f134c1d9bcb75d10d9098c5
出典データセット
uspto-grants-2004_06
特許番号
US06750218B2

関連ノート

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