反应详情

温度

50 °C

To a suspension of sodium hydride (5.2 gms.; 0.11 mole) (50% suspension mineral oil) in 100 ml of dry distilled DMF is added a solution of diethyl 1,4-dihydro-4-(2-trifluoromethylphenyl)-2,6-dimethyl-3,5-pyridine dicarboxylate (39.7 gms.; 0.1 mole) in 150 ml of DMF. After the gassing has ceased, the reaction mixture is heated on a water bath for 1 hour and then is cooled to 50° C. and to the hot solution is added a toluene solution of 2-chloro-N,N-bis(methoxyethyl)ethylamine. The reaction mixture is heated at 100°-110° C. for a period of 8 hours and then cooled. The unreacted NaH and NaCl is filtered off and the solvent removed from the filtrate. The residue is extracted with hot hexane which, on cooling, affords the desired product. Recrystallization from heptane yields the pure product.

1. customof dry
2. distillationdistilled DMF
3. temperaturethe reaction mixture is heated on a water bath for 1 hour
4. temperatureThe reaction mixture is heated at 100°-110° C. for a period of 8 hours
5. temperaturecooled
6. filtrationThe unreacted NaH and NaCl is filtered off
7. customthe solvent removed from the filtrate
8. extractionThe residue is extracted with hot hexane which
9. temperatureon cooling