反应详情

温度

60 °C

A stirred mixture of 4-hydroxy-alpha-oxobenzeneacetic acid methyl ester (0.724 g) in dimethylformamide (10 mL) under argon was treated with 55% sodium hydride (0.175 g), stirred for 15 minutes and treated with the mesylate of 2-(4-chlorophenoxy)ethanol (1.25 g). The mixture was heated at 60° C. overnight and worked up as in Example 20. The material from dichloromethane extraction was purified by HPLC (dichloromethane-hexane; 4:1 ) and crystallized from dichloromethane-hexane to provide 0.815 g of 4-[[2-(4-chlorophenoxy) ethyl]oxy]-alpha-oxobenzeneacetic acid methyl ester, mp 103°-105° C.

1. extractionThe material from dichloromethane extraction
2. customwas purified by HPLC (dichloromethane-hexane; 4:1 )
3. customcrystallized from dichloromethane-hexane