Sulfuric Acid → Estazolam

HRID 867066

反応式

HRID 867066 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 3261Estazolam

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-20254a603c274d94a25071f88736f4d1
出典データセット
uspto-grants-1978_07
特許番号
US04102881

関連ノート

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