Acetic Acid → alpha-(2-fluorophenyl)-N-t-butylnitrone

HRID 636721

反応式

HRID 636721 の反応式
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[CH3:10][C:11]([N+:14]([O-])=[O:15])([CH3:13])[CH3:12].C(O)(=O)C>C(O)C.[Zn]>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[N+:14]([C:11]([CH3:13])([CH3:12])[CH3:10])[O-:15]

参加物

6

反応物 3

HCID 176Acetic AcidHCID 116722-Methyl-2-nitropropaneHCID 67970o-Fluorobenzaldehyde

生成物 1

HCID 85599391alpha-(2-fluorophenyl)-N-t-butylnitrone

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

To a suspension of 2-fluorobenzaldehyde (332.3 mg, 2.68 mmol), 1,1-dimethylnitroethane (547.5 mg, 5.31 mmol) and zinc (514.6 mg, 7.87 mmol) in ethanol (3.0 ml) was added acetic acid (940.2 mg, 15.7 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 6.5 hours. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (hexane/ethyl acetate=4/1 to 2/1).

後処理

  1. stirringThe mixture was stirred at room temperature for 6.5 hours
  2. filtrationZinc acetate in the mixture was filtered off
  3. concentrationthe filtrate was concentrated
  4. custompurified by silica gel chromatography (hexane/ethyl acetate=4/1 to 2/1)

出典と根拠

ORDレコード
ord-61d658cb9eb749bda8fe13737e290f2a
出典データセット
uspto-grants-2001_02
特許番号
US06194461B1

関連ノート

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