Chloroform → 3beta-Acetoxy-5alpha,6beta-dichloro-14alpha-fluoropregnan-20-one

3β-Acetoxy-5α,6β-dichloropregnan-20-one (1.4g) was dissolved in fluorotrichloromethane (250 ml) and chloroform (200 ml) containing sodium trifluoroacetate (ca. 2g) and sodium fluoride (ca. 2g). The resulting solution was cooled to -78° and vigourously stirred, whereupon fluorine from four 750 cc bottles (10% v/v fluorine in nitrogen) was bubbled through the solution over a period of 8 hours. The reaction solution was then poured into aqueous sodium thiosulphate and the organic layer was separated, washed with water, dried over potassium carbonate and evaporated to dryness to yield crude 3β-acetoxy-5α,6β-dichloro-14α-fluoropregnan-20-one.

1. temperatureThe resulting solution was cooled to -78°
2. customwas bubbled through the solution over a period of 8 hours
3. additionThe reaction solution was then poured into aqueous sodium thiosulphate
4. customthe organic layer was separated
5. washwashed with water
6. dry with materialdried over potassium carbonate
7. customevaporated to dryness

ORD-Eintrag

ord-3c3ad565cd7d4aa7871d8411fd71edfe

Quelldatensatz

uspto-grants-1977_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04036864