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Dichloromethane → rac-7-amino-6,8-dichloro-5-(o-chlorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one

HRID 2199040
ノート
印刷プレビュー

反応式

HRID 2199040 の反応式
[Cl:1]N1C(=O)CCC1=O.[NH2:9][C:10]1C=[CH:12][C:13]2[N:19]([CH3:20])[C:18](=[O:21])[CH:17]([CH3:22])[N:16]=[C:15]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[Cl:29])[C:14]=2[CH:30]=1.[CH2:31]([Cl:33])Cl>C(=O)([O-])[O-].[Na+].[Na+]>[NH2:9][C:10]1[C:31]([Cl:33])=[CH:12][C:13]2[N:19]([CH3:20])[C:18](=[O:21])[CH:17]([CH3:22])[N:16]=[C:15]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[Cl:29])[C:14]=2[C:30]=1[Cl:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6344Dichloromethane2 回HCID 31398ChlorosuccinimideHCID 10335749rac-7-amino-5-(o-chlorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one

生成物 1

HCID 20516782rac-7-amino-6,8-dichloro-5-(o-chlorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one

試薬・触媒・溶媒 1

HCID 10340Sodium Carbonate溶媒

実験手順

26.8 g (0.2 mol) of N-chlorosuccinimide are added to a solution, stirred at room temperature, of 30 g (0.095 mol) of rac-7-amino-5-(o-chlorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one in 500 ml of methylene chloride and the mixture is stirred for 65 hours. The mixture is subsequently diluted with 400 ml of methylene chloride, 500 ml of 2 N sodium carbonate solution are added thereto, the phases are separated and the organic phase is washed with water. After drying and removal of the solvent in vacuo, the residue is chromatographed on 1 kg of silica gel using chloroform for the elution. From methylene chloride/cyclohexane there is obtained rac-7-amino-6,8-dichloro-5-(o-chlorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one of melting point 186°-187° C.

後処理

  1. additionare added
  2. customthe phases are separated
  3. washthe organic phase is washed with water
  4. customAfter drying
  5. customremoval of the solvent in vacuo
  6. customthe residue is chromatographed on 1 kg of silica gel
  7. washfor the elution

出典と根拠

ORDレコード
ord-2d7848c4d23a4ed5bb4c4f13f378b7f3
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04361511

反応ノート

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