反应详情

温度

92.5 °C

41 mL phenyl chloroformate are added dropwise to a solution of 47 g (183 mmol) 1-(3-amino-4-benzyloxy-2-hydroxy-phenyl)-ethanone (known from U.S. Pat. No. 4,460,581) in 135 mL pyridine, whereupon the temperature rises to 75° C. The mixture is stirred for 4 hours at 90-95° C., poured onto ice and acidified with hydrochloric acid. The precipitated solid is suction filtered, washed with diethyl ether and heated in 500 mL 95% acetonitrile for 30 minutes at reflux temperature. After cooling the solid is filtered off and washed with acetonitrile and diethyl ether.

1. customrises to 75° C
2. additionpoured onto ice
3. filtrationfiltered
4. washwashed with diethyl ether
5. temperatureheated in 500 mL 95% acetonitrile for 30 minutes
6. temperatureat reflux temperature
7. temperatureAfter cooling the solid
8. filtrationis filtered off
9. washwashed with acetonitrile and diethyl ether