Dimethylformamide → (+/-)-8-Methyl-5-(4-nitrophenyl)-7-(2-thiazolyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

HRID 25063

反応式

HRID 25063 の反応式
[CH3:1][CH:2]1[CH2:8][C:7]2[CH:9]=[C:10]3[O:15][CH2:14][O:13][C:11]3=[CH:12][C:6]=2[C:5]([C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=2)=[N:4][N:3]1[C:25](=[S:27])[NH2:26].[CH2:28](OC(OCC)CBr)[CH3:29].CN(C)C=O>O>[CH3:1][CH:2]1[CH2:8][C:7]2[CH:9]=[C:10]3[O:15][CH2:14][O:13][C:11]3=[CH:12][C:6]=2[C:5]([C:16]2[CH:17]=[CH:18][C:19]([N+:22]([O-:24])=[O:23])=[CH:20][CH:21]=2)=[N:4][N:3]1[C:25]1[S:27][CH:28]=[CH:29][N:26]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 74852Ethane, 2-bromo-1,1-diethoxy-HCID 12137394(+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

生成物 1

HCID 12137420(+/-)-8-Methyl-5-(4-nitrophenyl)-7-(2-thiazolyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 1.00 g (2.60 mmol) of the starting material I, 2.54 g (12.89 mmol) of bromoacetaldehyde diethyl acetal and 10 ml of dimethylformamide was stirred at 80° C. for 40 min. Then the reaction mixture was diluted with water and the crude product obtained was recrystallized from ethanol to yield 0.85 g (80%) of the title compound. Mp.: 145-150° C.

後処理

  1. customthe crude product obtained
  2. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-d6fbdcbbe9454367a6b64eb88f7e508c
出典データセット
uspto-grants-2005_02
特許番号
US06858605B2

関連ノート

読み込み中…