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

HRID 441487노트

반응식

HRID 441487 반응식
[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

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 12362349HCID 12362349, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e4a5ac633464381b699e0495e1b683e
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04041026

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