反应详情

To a suspension solution containing 4.4 g of 60% NaH in 200 ml of THF, 17.8 g of ethyl 3-phenylpropionate and 8.2 g of ethyl formate were added dropwise under ice cool for one hour. Thereafter, the mixture was stirred at room temperature for 15 hours. Furthermore, 14 g of 60 % NaH and 25.9 g of ethyl formate were divided into three parts and each part was added separately. Afterwards, the solution mixture was stirred at room temperature for 15 hours. After a 10% citric acid solution was added to the resultant reaction solution, the reaction solution was extracted with ethyl acetate and the extract was concentrated under reduced pressure to obtain 32.4 g of a brown oily concentrate. The concentrate thus obtained was purified by silica gel column chromatography to obtain 17.9 g of the titled compound as a transparent oily substance.

1. additionwere added dropwise under ice
2. temperaturecool for one hour
3. additioneach part was added separately
4. stirringAfterwards, the solution mixture was stirred at room temperature for 15 hours
5. customreaction solution
6. extractionthe reaction solution was extracted with ethyl acetate
7. concentrationthe extract was concentrated under reduced pressure
8. customto obtain 32.4 g of a brown oily concentrate
9. concentrationThe concentrate thus
10. customobtained
11. customwas purified by silica gel column chromatography