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

HRID 636721

반응식

HRID 636721 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-61d658cb9eb749bda8fe13737e290f2a
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194461B1

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