反应详情

In a three necked 1 liter round bottom reaction vessel equipped with a mechanical stirrer and reflux condenser were placed 48.8 g (0.15 mol) of the compound of Example 8 and 125 ml of hexamethylphosphorictriamide. The mixture was heated with stirring under nitrogen to 80°-85° C. To this solution 126 g (1.5 mol) of sodium bicarbonate powder was added portionwise followed by 20 g (0.17 mol) of allyl bromide. After 2.25 hours an additional 1.8 g (0.015 mol) of allyl bromide was added. After 29 hours of heating the reaction mixture was cooled to room temperature diluted with 700 ml of ethyl acetate, and the slurry was cross washed with water and diluted brine. The ethyl acetate was separated, dried with magnesium sulfate, clarified and taken to dryness under vacuum. The crude reaction mixture was crystallized from chloroform yielding 26.2 g of analytically pure product mp 99°-101° C.

1. customIn a three necked 1 liter round bottom reaction vessel equipped with a mechanical stirrer
2. temperaturereflux condenser
3. temperatureThe mixture was heated
4. temperatureAfter 29 hours of heating the reaction mixture
5. washthe slurry was cross washed with water and diluted brine
6. customThe ethyl acetate was separated
7. dry with materialdried with magnesium sulfate
8. customThe crude reaction mixture
9. customwas crystallized from chloroform yielding 26.2 g of analytically pure product mp 99°-101° C.