反应详情

To a mixture of (4-nitrophenoxy)acetic acid 22 (150 g, 761.4 mmol) and triethyl-amine (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)