(7α,17β)-3,17-Dihydroxy-7-[9-[(4,4,5,5,5-pentafluoropentyl)thio]nonyl]-estra-1,3,5(10)-trien-6-one synthesis

Yield:1107606-70-1 96.4%

Reaction Conditions:

with hydrogenchloride in ethanol at 0 - 10; for 2 h;Reagent/catalyst;Solvent;Temperature;

Steps:

1-1 Example 1-1

Compound III 5.0 g (6.5 mmol) was added to ethanol 50 mL, cooled to 0 °C,30% hydrogen chloride ethanol was added dropwise0.48 g (13 mmol) was added and the reaction was completed at 10 °C for 2.0 h.Treatment: Adjust pH=7 with triethylamine, concentrate under reduced pressure, add 50 mL of water, layer ethyl acetate 30 mL, extract the aqueous layer twice with ethyl acetate (30 mL×2), and wash the organic layer with 50 mL of water. Dry and evaporate to give compound IV 3.77g, yield 96.4%.

References:

CN107488205,2017,A Location in patent:Paragraph 0018; 0019; 0020; 0021; 0022