Ammonia → Clonazepam

HRID 725666

反応式

HRID 725666 の反応式
[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]

参加物

5

反応物 4

HCID 222AmmoniaHCID 1118Sulfuric Acid2 回HCID 24434Potassium NitrateHCID 145904461,3-Dihydro-5-(2-chlorophenyl)-2H-1,4-benzodiozepin-2-one

生成物 1

HCID 2802Clonazepam

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-ad0e7fb22a6a4b19a2c390a6a34d0ab0
出典データセット
uspto-grants-1998_01
特許番号
US05706829

関連ノート

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