反应详情

p-Methoxystyrene (40.8 g., 0.30 mole), 1,1-dichloro-2,2-difluoroethylene (55.8 g., 0.42 mole), and triethylamine (3.0 ml., 0.02 mole) are heated in a sealed tube (25 × 615 mm) at 125°-130° C. for 16 hrs. The cooled mixture is then poured into water, the reaction product extracted with ether, and the extracts washed with water, dried (MgSO4), and evaporated to an oil. Distillation of the oil yields 69.0 g. (86%), b.p. 80°-85° C. (0.1 mm), of the desired intermediate sutiable for use in the next step. Part of the oil was chromatographed (alumina, cyclohexane), and redistilled, b.p. 81° C. (0.02 mm), nD27 1.5207.

1. extractionthe reaction product extracted with ether
2. washthe extracts washed with water
3. dry with materialdried (MgSO4)
4. customevaporated to an oil
5. distillationDistillation of the oil
6. customyields 69.0 g
7. customPart of the oil was chromatographed (alumina, cyclohexane)
8. distillationredistilled