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

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

反応物 3

HCID 1118Sulfuric Acid

HCID 24261Silica

HCID 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).