反应详情

温度

0 °C

To a cooled solution (0° C.) of 5 ml. of 1 M borane in tetrahydrofuran in 2.7 ml. of dry tetrahydrofuran was added 500 mg. (1.4 millimole) of the product of Step C. in 2.0 ml. of dry tetrahydrofuran. The clear solution was stirred for 1 hr. at room temperature and then cooled to 0° C. and treated with 5 ml. of 2.5 N sodium hydroxide followed by 4 ml. of 30% hydrogen peroxide. The solution was stirred for 1 hr. at room temperature, diluted with water and extracted with ethyl ether, washed with water, brine, dried and evaporated to an oily crystalline material. The product was washed with cold methanol and pumped dry to give 175 mg. of final product having a m.p. of 167°-170° C.

1. customTo a cooled solution (0° C.) of 5 ml
2. additiontreated with 5 ml
3. stirringThe solution was stirred for 1 hr
4. extractionextracted with ethyl ether
5. washwashed with water, brine
6. customdried
7. customevaporated to an oily crystalline material
8. washThe product was washed with cold methanol
9. custompumped dry
10. customto give 175 mg