反应详情

A mixture of 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoic acid (7.24 g, 0.02 mole), ethylene carbonate (2.0 g, 0.023 mole) and tetraethylammonium iodide (1.0 g) was heated in an oil bath at 105°-110° C. for 10 hrs. The reaction was completed and the resulting gummy material was taken into 300 ml of ether. The ethereal solution was washed three times with water and dried over CaSO4. After the solvent had been removed, the product was crystallized from toluene/hexane and an almost quantitative yield (>95%) of the desired ester was obtained as a light brown crystalline solid; m.p. 71°-74° C., NMR (CDCl3) 3.33 (S, 1H), 3.67-4.12 (m, 2H), 4.15-4.63 (m, 2H), 7.02-8.25 (m, 6H); ir (CHCl3) 1749 cm-1. No by-product was detected by NMR analysis.

1. temperaturewas heated in an oil bath at 105°-110° C. for 10 hrs
2. washThe ethereal solution was washed three times with water
3. dry with materialdried over CaSO4
4. customAfter the solvent had been removed
5. customthe product was crystallized from toluene/hexane