反应详情

A mixture of 1,1-difluoro-2,2-dimethyl-3-(3-bromo-4-fluorobenzyloxy)propane (1.5 g), acetanilide (0.716 g), cuprous chloride (0.1 g); potassium carbonate (0.67 g), dry N,N-dimethylformamide (10 cm3) and tri[2-(2-methoxyethoxy)ethyl]amine (catalytic quantity) was heated at 158° C. for 4 days under an atmosphere of nitrogen; the mixture was then stood at the ambient temperature for 1 week. The combined organic extracts were washed with water and brine and dried over anhydrous magnesium sulphate. Evaporation of the solvent under reduced pressure gave a dark oil which was subjected to flash column chromatography on a silica gel support, eluting firstly with petroleum ether (boiling range 40°-6° C.) containing 2% by volume ethyl acetate (to give starting materials and a small amount of the deacylated product) and secondly with petroleum ether (boiling range 40°-60° C.) containing 50% by volume ethyl acetate, to give the title compound as a dark oil (0.68 g).

1. waitthe mixture was then stood at the ambient temperature for 1 week
2. washThe combined organic extracts were washed with water and brine
3. dry with materialdried over anhydrous magnesium sulphate
4. customEvaporation of the solvent under reduced pressure
5. customgave a dark oil which
6. washeluting firstly with petroleum ether (boiling range 40°-6° C.)
7. additioncontaining 2% by volume ethyl acetate (
8. customto give