反应详情

温度

40 °C

To a stirred mixture of methyl 3-(2-(4-morpholinophenylamino)pyrimidin-4-ylthio)benzoate (4.00 g, 9.46 mmol) in anhydrous tetrahydrofuran, was added lithium aluminum hydride (360 mg, 9.46 mmol) in small portions while the mixture was gently warmed to 40° C. The mixture was stirred at this temperature for about 4 hours. It was then cooled on an ice bath, cold 10% aqueous sodium bicarbonate solution was added slowly to quench the reaction. The whole mixture was partitioned between ethyl acetate and 10% aqueous sodium bicarbonate solution. The aqueous layer was re-extracted with ethyl acetate. The combined organic layer was washed with brine, dried (Na2SO4). Removal of the solvent in vacuo afforded the product (2.50 g, 80%).

1. temperatureIt was then cooled on an ice bath
2. customto quench
3. customthe reaction
4. customThe whole mixture was partitioned between ethyl acetate and 10% aqueous sodium bicarbonate solution
5. extractionThe aqueous layer was re-extracted with ethyl acetate
6. washThe combined organic layer was washed with brine
7. dry with materialdried (Na2SO4)
8. customRemoval of the solvent in vacuo