Methanol → HCID 22768399, 화합물

HRID 867064노트

반응식

HRID 867064 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 22768399HCID 22768399, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2a5a15a3c4e14cdab7e48d0bad45025c
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102881

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