Reaction #64739

Reaction equation

AlCl3

CF3CF2CF2OCF(CF3)COF

→

colorless liquid

CF3CF2CF2OCF(CF3)COCl

Solvents

o-dichlorobenzene

Conditions

Workup

1. 1
   OtherVolatiles were removed by vacuum transfer (27 Pa)
2. 2
   Otherto give
3. 3
   workup.ADDITIONa mixture of two liquids
4. 4
   OtherThe lower layer was separated
5. 5
   workup.DISTILLATIONdistilled

Procedure

A mixture of AlCl3 and o-dichlorobenzene (4 mL) was treated with CF3CF2CF2OCF(CF3)COF (13.2 g, 40 mmol) and heated at 60° C. for 0.5 hr. Volatiles were removed by vacuum transfer (27 Pa) to give a mixture of two liquids. The lower layer was separated and distilled to provide 8.0 g of colorless liquid, bp ca. 65° C. GC analysis showed 99% purity. 19F NMR (F11): -81.32 (s, CF3), -81.94 (t, J=7.3 Hz, CF3), -79.05 and -84.98 (AB pattern, J=146 Hz, OCF2), -126.1 (d of m's, J=23, CF), -130.1 (s, CF2).

Source