反应详情

温度

45 °C

A fresh solution of sodium diethyl phosphite was prepared from sodium hydride and diethyl phosphite in tetrahydrofuran at a concentration of 2 milliequivalents/ml and added, as described below, to a solution of 260 mg of 2,5-anhydro-2-C-[(phenylmethoxy)methyl]-3,4,6-tris-O-(phenylmethyl)-D-glucitol, 1-(trifluoromethanesulfonate) in 1 ml of tetrahydrofuran. A 0.5 ml portion of the stock solution was added and the mixture stirred 1.5 hours; 0.25 ml was added and stirring continued for 2.5 hours; 0.22 ml was added, the mixture warmed to 45° C. for 20 minutes then cooled to room temperature. The mixture was worked up with hexane, ether and water, giving an oil. This oil was purified by flash chromatography, eluting with 1% methanol in dichloromethane, giving 203 mg of the desired compound.

1. additionadded
2. additionA 0.5 ml portion of the stock solution was added
3. addition0.25 ml was added
4. stirringstirring
5. waitcontinued for 2.5 hours
6. addition0.22 ml was added
7. temperaturethen cooled to room temperature
8. customgiving an oil
9. customThis oil was purified by flash chromatography
10. washeluting with 1% methanol in dichloromethane