反应详情

First, 100 ml acrolein was added to a solution of 180 g diethyl bromomalonate, 14 g tributylamine, and 600 ml ethanol while cooling in an ice bath. After 2-3 hours, an additional 1.5 g tributylamine and 20 ml acrolein was added. The stirring was continued for an additional 1 to 2 hours without additional cooling. The reaction mixture was neutralized with 7 ml glacial acetic acid and the ethanol and unreacted acrolein were removed on a rotary evaporator. The residue was diluted with 500 ml benzene and washed with 3×100 ml H2O and 2×100 ml saturated NaCl solution. The benzene solution was dried over CaSO4 and rotary evaporated to yield 207 g of yellow oil which was indicated to be 48% product by glc.

1. temperaturewhile cooling in an ice bath
2. waitThe stirring was continued for an additional 1 to 2 hours without additional cooling
3. customthe ethanol and unreacted acrolein were removed on a rotary evaporator
4. additionThe residue was diluted with 500 ml benzene
5. washwashed with 3×100 ml H2O and 2×100 ml saturated NaCl solution
6. dry with materialThe benzene solution was dried over CaSO4
7. customrotary evaporated