HCID 21249960, 화합물 → HCID 21249961, 화합물

HRID 1531657노트

반응식

HRID 1531657 반응식
[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1>C(OC(=O)CC)(=O)CC.O>[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][N:9]([C:3](=[O:23])[CH2:2][CH3:22])[C:8]([CH3:21])=[CH:7][C:6]=2[CH:22]=1

참가 물질

4

반응물 1

HCID 21249960HCID 21249960, 화합물

생성물 1

HCID 21249961HCID 21249961, 화합물수율 140.3%

시약·촉매·용매 2

HCID 962Water용매HCID 31263Propionic anhydride용매

실험 절차

0.67 g (1.7 mmol) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is suspended in 3.35 ml of propionic acid anhydride and stirred for 3 hours at room temperature. The mixture is diluted with water, and the product is filtered. After washing with water and drying by column chromatography, the crude product is purified (silica gel, eluant benzene:ethyl acetate: 4:0.2). 0.53 g (70%) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-3-propionyl-3H-2,3-benzodiazepine is obtained as a thick oil.

후처리

  1. filtrationthe product is filtered
  2. washAfter washing with water
  3. customdrying by column chromatography
  4. customthe crude product is purified (silica gel, eluant benzene:ethyl acetate: 4:0.2)

출처 및 근거

ORD 기록
ord-157306b38e0f425792fb4a2f8c5c3672
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200970B1

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