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

HRID 35385

반응식

HRID 35385 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 13954659Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate수율 92.8%

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-988e1b0b73ce447b954125e277789977
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766238

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