Ammonia → Clonazepam

HRID 725666

반응식

HRID 725666 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:19])[CH2:10][N:9]=1.S(=O)(=O)(O)O.[N+:25]([O-])([O-:27])=[O:26].[K+].N>>[N+:25]([C:16]1[CH:17]=[CH:18][C:13]2[NH:12][C:11](=[O:19])[CH2:10][N:9]=[C:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[C:14]=2[CH:15]=1)([O-:27])=[O:26]

참가 물질

5

반응물 4

HCID 222AmmoniaHCID 1118Sulfuric Acid2회HCID 24434Potassium NitrateHCID 145904461,3-Dihydro-5-(2-chlorophenyl)-2H-1,4-benzodiozepin-2-one

생성물 1

HCID 2802Clonazepam

실험 절차

To a solution of 13.5 g. of 5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1H)-one in 60 ml. of concentrated sulfuric acid, a solution of 5.5 g. of potassium nitrate in 20 ml. concentrated sulfuric acid is added dropwise. The solution is then heated in a bath at 45-50° for 2 1/2 hours, cooled and poured on ice. After neutralizing with ammonia, the formed precipitate is filtered off and boiled with ethanol. A small amount of white insoluble material is then filtered off. The alcoholic solution on concentration yields crystals of 7-nitro-5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1H)-one (clonazepam) which, after recrystallization from dichloromethane, melt at 238-240°.

후처리

  1. temperatureThe solution is then heated in a bath at 45-50° for 2 1/2 hours
  2. temperaturecooled
  3. additionpoured on ice
  4. filtrationthe formed precipitate is filtered off
  5. filtrationA small amount of white insoluble material is then filtered off
  6. concentrationThe alcoholic solution on concentration

출처 및 근거

ORD 기록
ord-ad0e7fb22a6a4b19a2c390a6a34d0ab0
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05706829

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