HCID 21249960、化合物 → HCID 21249961、化合物

HRID 1531657ノート

反応式

HRID 1531657 の反応式
[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

参加物

4

反応物 1

HCID 21249960HCID 21249960、化合物

生成物 1

HCID 21249961HCID 21249961、化合物収率 140.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31263Propionic anhydride溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-157306b38e0f425792fb4a2f8c5c3672
出典データセット
uspto-grants-2001_03
特許番号
US06200970B1

反応ノート

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