Triethylamine → HCID 21249956、化合物

HRID 1531658ノート

反応式

HRID 1531658 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(N(CC)CC)C.[CH:32]1([C:35](Cl)=[O:36])[CH2:34][CH2:33]1>C(Cl)Cl>[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:35]([CH:32]3[CH2:34][CH2:33]3)=[O:36])[CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 21249960HCID 21249960、化合物

生成物 1

HCID 21249956HCID 21249956、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.69 g (1.77 mmol) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is acylated in methylene chloride (15 ml) in the presence of 0.29 ml (2.1 mmol) of triethylamine with 0.19 ml (2.1 mmol) of cyclopropanoic acid chloride at room temperature for 1.5 hours. After concentration by evaporation and suspension with water, 0.78 g of a crude product, which is purified by suspension in hot ethanol, is obtained. 0.75 g (93%) of 7-bromo-3-cyclopropylcarbonyl-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine with a melting point of 194-196° C. is obtained.

後処理

  1. concentrationAfter concentration
  2. customby evaporation and suspension with water, 0.78 g of a crude product, which
  3. customis purified by suspension in hot ethanol
  4. customis obtained

出典と根拠

ORDレコード
ord-7c60cf63ded243b0bfd61274c4f0a350
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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