反应详情

718 mg of methylamine are condensed at −78° C. into a solution of 960 mg of 11β-fluoro-3-hydroxy-7α-(6-iodo-hexyl)oestra-1,3,5(10)-trien-17-one in 9 ml of anhydrous tetrahydrofuran and the mixture is stirred overnight at room temperature in a pressure reactor. After the pressure reactor has been opened at −20° C., it is allowed to come to room temperature in order to allow excess methylamine to evaporate. The reaction solution is then added to saturated sodium hydrogencarbonate solution, extracted 3 times with ethyl acetate, dried over sodium sulphate and concentrated in vacuo. 763 mg of 11β-fluoro-3-hydroxy-7α-[5-(methylamino)hexyl]oestra-1,3,5(10)-trien-17-one are obtained as a crude product.

1. customhas been opened at −20° C.
2. customto come to room temperature in order
3. customto evaporate
4. additionThe reaction solution is then added to saturated sodium hydrogencarbonate solution
5. extractionextracted 3 times with ethyl acetate
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated in vacuo