反应详情

To a solution of 420 mG of 60% sodium hydride dispersion (0.011 mol), 6.26 g (0.01 mol) of N,N-dioctadecylaminobenzaldehyde and 40 mL of dry, freshly distilled 1,2-dimethoxyethane (DME) under nitrogen, at room temperature, with vigorous stirring, was added a solution of 3.06 g (0.01 mol) of diethyl 4-methylsulfonylbenzylphosphonate in 10 mL 1,2-dimethoxyethane. The mixture immediately turned bright yellow. The reaction mixture was heated at reflux for 2 hours. After cooling, the bright yellow solution was poured over 100 g of crushed ice under a nitrogen blanket. The bright yellow solid was collected by filtration, washed with cold water, and air dried. Recrystallization from ethanol yielded 3.95 g (50.7%) of bright yellow powder mp 75°-76° C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 hours
3. temperatureAfter cooling
4. filtrationThe bright yellow solid was collected by filtration
5. washwashed with cold water, and air
6. customdried
7. customRecrystallization from ethanol