Steroid conjugates. Part I. Syntheses of 5β-pregnane-3α20α-diol sulphates

Abstract

Sulphation of 5β-pregnane-3α,20α-diol with an excess of chlorosulphonic acid in pyridine gives the corresponding disulphate, While one molar equivalent of the reagent leads to a mixture of the 3- and 20-monosulphates. The 3-monosulphate has been prepared via the 20-monoacetate. Water of cristallisation in these conjugates is readily detected by n.m.r. spectroscopy, integrated intensities being consisten with microanalyses for a variety of salts.