反应详情

Add [dropwise, with stirring, at from 90°-100°, in a stream of nitrogen] a solution of 5.1 g of sodium in 100 ml of ethanol to a mixture of 32 g of 4-chlorophenylacetic acid ethyl ester and 59.13 g of 1-isopropyl-2-dimethylamino-1-pyrrolinium-methylsulfate. After completion of the addition, continue stirring for a further 30 minutes; then cool and take up with water (≈100 ml) and diethyl ether (≈150 ml). Collect the organic phase, extract the aqueous phase once again with diethyl ether, combine the ether extracts, dry and concentrate them to obtain a yield [45.6 g (92% of theory)] of crude title compound; recrystallize 5 g from ethanol/water to obtain 4.2 g of product with a m.p. of 70° to 71°.

1. additionAdd [dropwise,
2. additionAfter completion of the addition
3. temperaturethen cool
4. customCollect the organic phase
5. extractionextract the aqueous phase once again with diethyl ether
6. customdry
7. concentrationconcentrate them
8. customto obtain
9. customa yield [45.6 g (92% of theory)] of crude title compound
10. customrecrystallize 5 g from ethanol/water