Acetic Anhydride → N,3-bis-(4-chlorophenyl)-4-dimethylcarbamoyl-4-methyl-N-acetyl-4,5-dihydro-1H-pyrazole-1-carboxamide

HRID 978171ノート

反応式

HRID 978171 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([N:13]2[CH2:17][C:16]([C:19](=[O:23])[N:20]([CH3:22])[CH3:21])([CH3:18])[C:15]([C:24]3[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1.[H][H].[C:33](OC(=O)C)(=[O:35])[CH3:34]>O1CCCC1>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]([C:33](=[O:35])[CH3:34])[C:11]([N:13]2[CH2:17][C:16]([C:19](=[O:23])[N:20]([CH3:22])[CH3:21])([CH3:18])[C:15]([C:24]3[CH:25]=[CH:26][C:27]([Cl:30])=[CH:28][CH:29]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 7918Acetic AnhydrideHCID 24758Sodium hydrideHCID 13825589N,3-bis-(4-chlorophenyl)-4-dimethylcarbamoyl-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 53786372N,3-bis-(4-chlorophenyl)-4-dimethylcarbamoyl-4-methyl-N-acetyl-4,5-dihydro-1H-pyrazole-1-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In a 50 ml round bottomed flask was placed 0.45 g of 60% sodium hydride (0.011 mole). The sodium hydride was washed twice with hexane and suspended in 15 ml of tetrahydrofuran. A solution of 2.0 g (0.005 mole) of N,3-bis-(4-chlorophenyl)-4-dimethylcarbamoyl-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide in 5 ml of tetrahydrofuran was added slowly. When hydrogen evolution ceased, 1 ml of acetic anhydride was added and the mixture was stirred for 5 minutes. The reaction was partitioned between ethyl ether and brine, dried, concentrated, and chromatographed yielding 1.6 g of N,3-bis-(4-chlorophenyl)-4-dimethylcarbamoyl-4-methyl-N-acetyl-4,5-dihydro-1H-pyrazole-1-carboxamide, an oil. NMR and IR data were consistent with the structure.

後処理

  1. customIn a 50 ml round bottomed flask was placed
  2. washThe sodium hydride was washed twice with hexane
  3. customThe reaction was partitioned between ethyl ether and brine
  4. customdried
  5. concentrationconcentrated
  6. customchromatographed

出典と根拠

ORDレコード
ord-1a954d2aff614ae7812c308ef01ffec3
出典データセット
uspto-grants-1987_05
特許番号
US04663341

反応ノート

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