Triethylamine → 5-Methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-one

HRID 441487ノート

反応式

HRID 441487 の反応式
[N+]([N:4]1[C:10]([O:17][CH3:18])([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]2[CH:19]=[C:20]([N+:23]([O-:25])=[O:24])[CH:21]=[CH:22][C:8]=2[N:7]([CH3:26])[C:6](=[O:27])[CH2:5]1)([O-])=O.C(N(CC)CC)C>C(Cl)Cl>[CH3:18][O:17][C:10]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]2[CH:19]=[C:20]([N+:23]([O-:25])=[O:24])[CH:21]=[CH:22][C:8]=2[N:7]([CH3:26])[C:6](=[O:27])[CH:5]=[N:4]1

参加物

4

反応物 2

HCID 8471TriethylamineHCID 12362349HCID 12362349、化合物

生成物 1

HCID 439385-Methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-one収率 56.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 4.7-dinitro-5-methoxy-1-methyl-5-phenyl-1,3,4,5-tetrahydro-2H-1,4-benzodiazepin-2-one (400 mg) and triethylamine (1.1 g) in methylene chloride (10 ml) is allowed to stand at room temperature for 72 hours. The reaction mixture is washed with water, dried over sodium sulfate, and evaporated under reduced pressure to remove the solvent. The residue is washed with diethyl ether to give 5-methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-one (196 mg) as crude product.

後処理

  1. washThe reaction mixture is washed with water
  2. dry with materialdried over sodium sulfate
  3. customevaporated under reduced pressure
  4. customto remove the solvent
  5. washThe residue is washed with diethyl ether

出典と根拠

ORDレコード
ord-6e4a5ac633464381b699e0495e1b683e
出典データセット
uspto-grants-1977_08
特許番号
US04041026

反応ノート

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