Methanol → HCID 22768399、化合物

HRID 867064ノート

反応式

HRID 867064 の反応式
C(O[C:4]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:6]=2[N:5]=1)C.CO.O.[NH2:27][NH2:28]>O>[NH:27]([C:4]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:6]=2[N:5]=1)[NH2:28]

参加物

5

反応物 3

HCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 203172642-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine

生成物 1

HCID 22768399HCID 22768399、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 0.25 part of 2-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine in 8 parts by volume of methanol is added 0.2 part by volume of hydrazine hydrate (100%) with stirring and the stirring is continued at room temperature for further 2.5 hours. To the reaction mixture is added water, followed by extraction with chloroform. Chloroform layer is washed with water and dried over anhydrous sodium sulfate, followed by distillation of the solvent. Treatment of the residue with n-hexane gives 2-hydrazino-7-nitro-5-phenyl-3H-1,4-benzodiazepine as orange crystalline powder. The product is treated with acetone, whereupon 2-(2-isopropylidenehydrazino)-7-nitro-5-phenyl-3H-1,4-benzodiazepine is obtained as pale yellow crystals melting at 203°-205° C.

後処理

  1. extractionfollowed by extraction with chloroform
  2. washChloroform layer is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationfollowed by distillation of the solvent

出典と根拠

ORDレコード
ord-2a5a15a3c4e14cdab7e48d0bad45025c
出典データセット
uspto-grants-1978_07
特許番号
US04102881

反応ノート

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