Chloroacetyl chloride → dimethyl 5-(chloroacetyl)-13-cyclohexyl-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-6,10-dicarboxylate

HRID 1518222ノート

反応式

HRID 1518222 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[CH:6]1([C:12]2[C:13]3[CH:14]=[CH:15][C:16]([C:34]([O:36][CH3:37])=[O:35])=[CH:17][C:18]=3[N:19]3[C:25]=2[C:24]2[CH:26]=[CH:27][CH:28]=[CH:29][C:23]=2[NH:22][CH:21]([C:30]([O:32][CH3:33])=[O:31])[CH2:20]3)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1>CCOC(C)=O>[Cl:1][CH2:2][C:3]([N:22]1[C:23]2[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=2[C:25]2=[C:12]([CH:6]3[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]3)[C:13]3[CH:14]=[CH:15][C:16]([C:34]([O:36][CH3:37])=[O:35])=[CH:17][C:18]=3[N:19]2[CH2:20][CH:21]1[C:30]([O:32][CH3:33])=[O:31])=[O:4]

参加物

4

反応物 2

HCID 6577Chloroacetyl chlorideHCID 66673930dimethyl 13-cyclohexyl-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-6,10-dicarboxylate

生成物 1

HCID 68708149dimethyl 5-(chloroacetyl)-13-cyclohexyl-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-6,10-dicarboxylate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

Chloroacetyl chloride (5 eq) was added to a sealed tube containing dimethyl 13-cyclohexyl-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-6,10-dicarboxylate (1 eq.). The mixture was heated at 40° C. overnight. The mixture was allowed to cool to RT before being diluted with EtOAc and washed with saturated aqueous NaHCO3 and brine. The organic phase was dried over sodium sulfate, filtered and evaporated in vacuo to afford the title compound (quant.). MS (ES+) m/z 509 (M+H)+.

後処理

  1. temperatureto cool to RT
  2. washwashed with saturated aqueous NaHCO3 and brine
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-5c018ae5d212428ea2e570d54bc91dba
出典データセット
uspto-grants-2012_07
特許番号
US08232390B2

反応ノート

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