Sulfuric Acid → Estazolam

HRID 867066노트

반응식

HRID 867066 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.[CH:21]([O-])([O-])OCC.S(=O)(=O)(O)O.C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:21]=[N:13][N:12]=[C:10]3[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepineHCID 53630039Ethylorthoformate

생성물 1

HCID 3261Estazolam

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 2.0 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine and 7.4 parts of ethyl orthoformate in 80 parts by volume of chloroform is added 2 parts of concentrated sulfuric acid with stirring. The mixture is stirred at room temperature for further 30 minutes, and neutralized with a saturated aqueous sodium bicarbonate solution. Chloroform layer is washed with water and dried over sodium sulfate, followed by distillation of the solvent. Recrystallization of the residue from acetone-n-hexane yields 8-chloro-6-phenyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepine as colorless flakes melting at 226°-227° C.

후처리

  1. stirringThe mixture is stirred at room temperature for further 30 minutes
  2. washChloroform layer is washed with water
  3. dry with materialdried over sodium sulfate
  4. distillationfollowed by distillation of the solvent
  5. customRecrystallization of the residue from acetone-n-hexane

출처 및 근거

ORD 기록
ord-20254a603c274d94a25071f88736f4d1
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102881

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