1,2-Dibromoethane → HCID 20735779, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 16.4 g (0.25 mol) of zinc dust, 200 mL of dry DMF, and 2 mL of 1,2-dibromoethane was stirred under N2 while a small portion of 41 g (0.112 mol) of 20 was added. The mixture was heated until reaction had started (ca. 90° C.), then the remainder of 20 was added dropwise at a rate sufficient to maintain temperature up to 105° C. in the pot while product was taken overhead as formed, bp 60°-65° C. When the addition had been completed, the pot temperature was increased until distillate was being collected at 135° C. The distillate was washed with water, dried over CaSO4, filtered and distilled to afford 14.2 g (43%) of perfluoro-2,3-dimethyl-2,3-dihydro-1,4-dioxin (21), bp 65°-67.5° C.

Provenance & Evidence