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

HRID 258185

反応式

HRID 258185 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 14695235Ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate収率 87%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

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-methyl-cyclopropane-carboxylate are obtained in form of a liquid of boiling point 141°-143° C.

後処理

  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

出典と根拠

ORDレコード
ord-4508dfb168c9441fa93e28d42cbd2758
出典データセット
uspto-grants-1993_11
特許番号
US05264632

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