A process for obtaining a 21-disodium phosphate pregnane compd. comprises spray drying a soln. contg. this compd. Prednisolone 21-disodium phosphate with a purity of 98.4% was dissolved water to give a 5% soln. The pH of the soln. was adjusted to 7.6/7.9 by addn. of 1N HCl. The product, prednisolone 21-phosphate was obtained with a purity of 99.2%.