反应详情

NaH (4.8 grams in a 50% oil dispersion) was placed in a 500 ml. 3-necked flask under an atmosphere of nitrogen and, after the addition of 80 ml. of THF, the mixture was heated to reflux. Next a solution of ethyl-3-(trifluoromethyl)benzoate (19 grams), acetonitrile, (5 grams) and THF (20 ml.) was added. Reflux was continued for 2 hours and then the reaction mixture was cooled and 250 ml. ether added. The organic layer was first extracted with 1 N NaOH, and then washed with brine and dried. Removal of the solvent afforded 11 grams of solid product, m.p. 58°-60° C.

1. addition3-necked flask under an atmosphere of nitrogen and, after the addition of 80 ml
2. temperatureReflux
3. temperaturethe reaction mixture was cooled
4. extractionThe organic layer was first extracted with 1 N NaOH
5. washwashed with brine
6. customdried
7. customRemoval of the solvent