Water → HCID 21249983、化合物

HRID 1531656ノート

反応式

HRID 1531656 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][N:9]=[C:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1.C(=O)([O-])[O-].[K+].[K+].[CH:31]1([C:34](Cl)=[O:35])[CH2:33][CH2:32]1.O>C1C=CC=CC=1>[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:34]([CH:31]3[CH2:33][CH2:32]3)=[O:35])[C:8]([CH3:21])=[CH:7][C:6]=2[CH:22]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 77637Cyclopropanecarbonyl chlorideHCID 21249973HCID 21249973、化合物

生成物 1

HCID 21249983HCID 21249983、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

0.5 g of 7-bromo-1-(4-nitrophenyl)-4-methyl-8-methoxy-5H-2,3-benzodiazepine (Example 3, Step C) is suspended in 15 ml of benzene, mixed with 0.53 g of potassium carbonate and 0.17 ml of cyclopropylcarboxylic acid chloride and then refluxed for 5 hours. Then, the mixture is stirred with water, the organic phase is separated, washed in succession with soda solution and water, dried, filtered and concentrated by evaporation. The residue is purified by absorptive precipitation in ethanol, and 0.38 g of 7-bromo-3-cyclopropylcarbonyl-1-(4-nitrophenyl)-4-methyl-8-methoxy-3H-2,3-benzodiazepine of the title compound with a melting point of 231-223° C. is obtained.

後処理

  1. temperaturerefluxed for 5 hours
  2. customthe organic phase is separated
  3. washwashed in succession with soda solution and water
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customThe residue is purified by absorptive precipitation in ethanol

出典と根拠

ORDレコード
ord-6d546301daec4266a05d92c60bc47078
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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