反应详情

Trifluoroacetic anhydride (8.4 g, 0.04 mole) was added portionwise to a solution of 2-hydroxyethyl 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate (7 g, 0.017 mole) and 50 ml of ether. After holding at 30°-35° C. for an hour, the solution was allowed to stand at room temperature overnight. Excess trifluoroacetic anhydride was removed and 300 ml of ether was added. The ethereal solution was washed three times with water, dried over CaSO4 and concentrated to an oil. Kugelrohr distillation afforded 3.6 g of pure 2-(trifluoroacetoxy)ethyl 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate as a gumming material (yield: 42.2%); nmr (CDCl3) δ 4.62 (s, 4H), 7.02-8.19 (m, 6H); ir (CHCl3) 1752, 1803 Cm-1.

1. waitAfter holding at 30°-35° C. for an hour
2. customExcess trifluoroacetic anhydride was removed
3. addition300 ml of ether was added
4. washThe ethereal solution was washed three times with water
5. dry with materialdried over CaSO4
6. concentrationconcentrated to an oil
7. distillationKugelrohr distillation