Ethanol → Ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate

HRID 248220

반응식

HRID 248220 반응식
[F:1][C:2]1([F:9])[CH2:4][C:3]1([CH3:8])[C:5](Cl)=[O:6].[CH2:10]([OH:12])[CH3:11]>S(=O)(=O)(O)O>[F:1][C:2]1([F:9])[CH2:4][C:3]1([CH3:8])[C:5]([O:12][CH2:10][CH3:11])=[O:6]

참가 물질

4

반응물 2

HCID 702EthanolHCID 146952322,2-Difluoro-1-methylcyclopropane-1-carbonyl chloride

생성물 1

HCID 14695235Ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate수율 87%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

35 ml of ethanol are added dropwise at 20° C. to 15.45 g (0.1 mol) of 2,2-difluoro-1-methyl-cyclopropanecarbonyl chloride, with stirring. After the addition of 2 drops of concentrated sulphuric acid, the reaction mixture is refluxed for another hour. Excess ethanol is subsequently distilled off, and the residue is dried and distilled under atmospheric pressure. In this manner, 14.2 g (87% of theory) of ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate are obtained in form of a liquid of boiling point 141°-143° C.

후처리

  1. temperaturethe reaction mixture is refluxed for another hour
  2. distillationExcess ethanol is subsequently distilled off
  3. customthe residue is dried
  4. distillationdistilled under atmospheric pressure

출처 및 근거

ORD 기록
ord-2a6031f8ea2b4a4e9ac3f342e3a8cf70
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05208388

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