四氧化硫 → Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate

HRID 35385

反应方程式

HRID 35385 反应方程式
[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]

参与物

4

反应物 3

HCID 1118四氧化硫HCID 24261Fumed silicaHCID 138276951-Chloromethoxy-1,1-difluoro-2-trifluoromethyl-3,3,3-trifluoropropane

产物 1

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

实验过程

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).

后处理

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

来源与证据

ORD记录
ord-988e1b0b73ce447b954125e277789977
来源数据集
uspto-grants-1988_08
专利号
US04766238

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