反应详情

10 g of 3-phenoxybenzaldehyde cyanohydrin were added dropwise to a mixture of 5.1 g of lithium aluminum hydride and 500 ml of tetrahydrofuran, whilst ice-cooling, and the resulting mixture was heated under reflux for 4 hours. At the end of this time, 5 ml of water, 6 ml of a 15% w/v aqueous solution of sodium hydroxide and 18 ml of water were added in that order to the reaction mixture, whilst ice-cooling. Insoluble materials were filtered off, and the filtrate was concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, using a 3:1 by volume mixture of ethyl acetate and ethanol as the eluent, to give the title compound having an Rf=0.32 (thin layer chromatography over silica gel, using a 5:5:1 by volume mixture of ethyl acetate, ethanol and triethylamine as the developing solvent).

1. temperaturecooling
2. temperaturethe resulting mixture was heated
3. temperatureunder reflux for 4 hours
4. temperaturecooling
5. filtrationInsoluble materials were filtered off
6. concentrationthe filtrate was concentrated by evaporation under reduced pressure
7. customThe concentrate was purified by column chromatography through silica gel
8. additionby volume mixture of ethyl acetate and ethanol as the eluent