Acetic Acid → HCID 73197187、化合物

HRID 636725

反応式

HRID 636725 の反応式
[CH3:1][C:2]([N+:5]([O-:7])=O)([CH3:4])[CH3:3].C(O)(=O)C.[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1>C(O)C.[Zn]>[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=[N+:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[O-:7])=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 116722-Methyl-2-nitropropaneHCID 7365304-(1H-imidazol-1-yl)benzaldehyde

生成物 1

HCID 73197187HCID 73197187、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

反応条件

温度
5 °C

実験手順

To a suspension of 1,1-dimethylnitroethane (261.2 mg, 2.53 mmol) and zinc (247.0 mg, 3.78 mmol) in ethanol (3.0 ml) was added acetic acid (451.8 mg, 7.52 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 30 minutes. After cooling the mixture to 5° C. again, 4-(1-imidazolyl)benzaldehyde (216.5 mg, 1.26 mmol) was added dropwise to the mixture while stirring and stirred at room temperature overnight. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (chloroform/methanol=10/1).

後処理

  1. stirringThe mixture was stirred at room temperature for 30 minutes
  2. stirringwhile stirring
  3. stirringstirred at room temperature overnight
  4. filtrationZinc acetate in the mixture was filtered off
  5. concentrationthe filtrate was concentrated
  6. custompurified by silica gel chromatography (chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-bda5bfc6fee9495a97edd7e3f247ff2e
出典データセット
uspto-grants-2001_02
特許番号
US06194461B1

関連ノート

読み込み中…