Dimethylformamide → 7-Chloro-5-phenyl-1,2,3,4-tetrahydro-2-nitromethylene-5H-1, 5-benzodiazepin-4-one

HRID 1679288ノート

反応式

HRID 1679288 の反応式
CC(C)([O-])C.[K+].CN(C)C=O.[N+:12]([CH3:15])([O-:14])=[O:13].[Cl:16][C:17]1[CH:38]=[CH:37][C:20]2[N:21]=[C:22](NCN=O)[CH2:23][C:24](=[O:32])[N:25]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:19]=2[CH:18]=1>O.C(O)(=O)C>[Cl:16][C:17]1[CH:38]=[CH:37][C:20]2[NH:21][C:22](=[CH:15][N+:12]([O-:14])=[O:13])[CH2:23][C:24](=[O:32])[N:25]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:19]=2[CH:18]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6375NitromethaneHCID 23665647Potassium tert-butoxideHCID 1785263748-chloro-4-(nitrosomethylamino)-1-phenyl-3H-1,5-benzodiazepin-2-one

生成物 1

HCID 706056287-Chloro-5-phenyl-1,2,3,4-tetrahydro-2-nitromethylene-5H-1, 5-benzodiazepin-4-one

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

Potassium t-butoxide, 10.24 g (.092 moles) was added to a mixture of 250 ml of dimethylformamide and 50 ml of nitromethane. After stirring at room temperature for 15 min under nitrogen, 25 g (0.076 m) of 7-chloro-3,5-dihydro-2-(N-nitrosomethylamino)-5-phenyl-4H-1,5-benzodiazepin-4-one was added and stirring was continued for an additional 19 hours. The mixture was acidified with acetic acid and diluted with water. The precipitate was filtered off, washed with water and recrystallized from methylene chloride/ethanol to give pale yellow crystals with mp 259°-261°.

後処理

  1. stirringstirring
  2. waitwas continued for an additional 19 hours
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customrecrystallized from methylene chloride/ethanol
  6. customto give pale yellow crystals with mp 259°-261°

出典と根拠

ORDレコード
ord-1d3c4d45d37e405cbd644ac423749511
出典データセット
uspto-grants-1978_03
特許番号
US04080323

反応ノート

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