反应详情

To a solution of 2.8 g (0.07 mol) of 60% sodium hydride dispersion, 7.46 g (0.05 mole) N,N-dimethylaminobenzaldehyde, and 100 mL of dry, freshly distilled 1,2-dimethoxyethane (DME) under nitrogen, at room temperature, was added 15.3 g (0.05 mole) diethyl 4-methylsulfonylbenzylphosphonate with vigorous stirring. The mixture immediately turned bright yellow. The mixture was heated at reflux for 2 hours. After cooling the very bright yellow solution was poured over 300 g of crushed ice under nitrogen blanket. The bright yellow solid was collected by filtration, washed with water, and air dried. Recrystallization from a 1:1 mixture of absolute ethanol and dry pyridine yielded 9.97 g (66%) of bright yellow crystals mp 242°-243° C.

1. temperatureThe mixture was heated
2. temperatureat reflux for 2 hours
3. temperatureAfter cooling the very bright yellow solution
4. filtrationThe bright yellow solid was collected by filtration
5. washwashed with water, and air
6. customdried
7. customRecrystallization
8. additionfrom a 1:1 mixture of absolute ethanol and dry pyridine