Silica → Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate

HRID 35387

Reaction equation

HRID 35387 reaction equation
[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(F)(=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]

Participants

4

Reactant 3

HCID 24261SilicaHCID 24603Fluorosulfuric acidHCID 138276951-Chloromethoxy-1,1-difluoro-2-trifluoromethyl-3,3,3-trifluoropropane

Product 1

HCID 13954659Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate

Procedure

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), silicon dioxide and fluorosulfuric acid (70.0 g, 0.70 mol) were charged. 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 (190.3 g).

Workup

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

Sources & evidence

ORD record
ord-3e95dee8e9c04b8297e0607bbde36700
Source dataset
uspto-grants-1988_08
Patent number
US04766238

Linked notes

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