反应详情

To a mixture of (4-nitrophenoxy) acetic acid 22 (150 g, 761.4 mmol) and triethylamine (85 g, 840 mmol) in acetone (750 ml) was added methyl chloroacetate (91.6 g, 844 mmol) drop wise and stirred under reflux for 8 hours. Solids were filtered off and poured onto cold 5% sodium bicarbonate solution (4 L). Crude 44 was filtered, dried and recrystallised from chloroform:hexane (1:6) to get pure 44 (186 g, 90.8%) as a white powder with an m.p. between 88-90° C.

1. temperatureunder reflux for 8 hours
2. filtrationSolids were filtered off
3. additionpoured onto cold 5% sodium bicarbonate solution (4 L)
4. filtrationCrude 44 was filtered
5. customdried
6. customrecrystallised from chloroform:hexane (1:6)