反应详情

温度

100 °C

A mixture of 0.70 g of the phenol compound(prepared as described in Example 9), 0.30 g of sodium hydride (content 63%) and 14 ml of N,N-dimethylformamide was stirred at 100° C. for 20 minutes, and stirred with 0.64 g of ethyl bromoacetate at 70° C. for 2 hours. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in water, and extracted with diethyl ether. The extract was washed with water, and a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a 0.5% V/V solution of ethanol in chloroform as eluent to give 0.166 g of the title compound having the following physical characteristics:

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionthe residue was dissolved in water
3. extractionextracted with diethyl ether
4. washThe extract was washed with water
5. dry with materiala saturated aqueous solution of sodium chloride, dried over sodium sulphate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel using a 0.5% V/V solution of ethanol in chloroform as eluent