Sulfuric Acid → Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate

HRID 35385

反応式

HRID 35385 の反応式
[Cl:1][CH2:2][O:3][C:4](F)(F)[CH:5]([C:10]([F:13])([F:12])[F:11])[C:6]([F:9])([F:8])[F:7].[Si](=O)=[O:17].S(=O)(=O)(O)O>>[F:7][C:6]([F:9])([F:8])[CH:5]([C:10]([F:13])([F:12])[F:11])[C:4]([O:3][CH2:2][Cl:1])=[O:17]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 24261SilicaHCID 138276951-Chloromethoxy-1,1-difluoro-2-trifluoromethyl-3,3,3-trifluoropropane

生成物 1

HCID 13954659Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate収率 92.8%

実験手順

In a four necked 1 liter flask equipped with a thermometer, a condenser and a stirrer, 1-chloromethoxy-1,1-difluoro-2-trifluoromethyl-3,3,3-trifluoropropane (276.6 g, 1.04 mol) and silicon dioxide (50.8 g, 0.85 mol) were charged, and concentrated sulfuric acid (60 g, 0.61 mol) was dropwise added thereto while stirring. The reaction was continued at 110° C. for 21 hours. Then, the reaction mixture was distilled to give monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (192.9 g).

後処理

  1. additionwere charged
  2. distillationThen, the reaction mixture was distilled

出典と根拠

ORDレコード
ord-988e1b0b73ce447b954125e277789977
出典データセット
uspto-grants-1988_08
特許番号
US04766238

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