反应详情

5.1 g of methylamine is condensed in a solution of 6.8 g of 11β-fluoro-3-hydroxy-7α-(5-iodopentyl)-estra-1,3,5(10)-trien-17-one in 35 ml of anhydrous tetrahydrofuran at −78° C., and it is stirred overnight at room temperature in a pressurized reactor. After the pressurized reactor was opened at −20° C., it is allowed to come to room temperature to allow excess methylamine to evaporate off. Then, the reaction solution is added to saturated sodium bicarbonate solution, extracted 3 times with ethyl acetate, dried on magnesium sulfate and concentrated by evaporation in a vacuum. 6.7 g of 11β-fluoro-3-hydroxy-7α-[5-(methyl-amino)-pentyl]-estra-1,3,5(10)-trien-17-one is obtained as a crude product.

1. customwas opened at −20° C.
2. customto come to room temperature
3. customto evaporate off
4. additionThen, the reaction solution is added to saturated sodium bicarbonate solution
5. extractionextracted 3 times with ethyl acetate
6. customdried on magnesium sulfate
7. concentrationconcentrated by evaporation in a vacuum