Zeranol production
AssigneeC.R.C. Compagnia di Ricera Chimica S.p.A.
InventorsFlavio Moimas, Giuliano Clauti
Life of this patent
Estimating the term…
Abstract
A process for producing high purity .alpha.-zeranol from a zeralenone containing surface fermentation product is described. One feature of the process entails fractional crystallization from an aqueous acetonitrile solvent of high purity .alpha.-zeranol from a solution containing a mixture of 50 to 60 parts by weight .alpha.-zeranol and 40 to 50 parts by weight .beta.-zeranol.
Claims3
In a process for the production of .alpha.-zeranol of high purity from a first mixture of .alpha. and .beta. zeranol containing from out 50% to about 60% by weight of .alpha.-zeranol in which a second mixture of .alpha. and .beta. zeranol containing less than 50% by weight of .alpha.-zeranol is produced, the improvement which comprises:
- (i) subjecting said second mixture to dehydrogenation in the presence of Raney nickel in an n-butyl acetate medium and terminating said dehydrogenation at a conversion of about 75% to about 80% to provide a dehydrogenation product consisting essentially of zeralanone and a third mixture of .alpha. and .beta. zeranol containing more than 50% .alpha.-zeranol;
- and
- (ii) hydrogenating said dehydrogenation product with zeralenone in the presence of Raney nickel in a water methanol medium to provide a fourth mixture of .alpha. and .beta. zeranol the .alpha.-zeranol content of said fourth mixture being greater than the .alpha.-zeranol content of said third mixture.
In a process for recovering a mixture of crystalline zeralanone, .alpha.-zeranol and .beta.-zeranol from a mother liquor which results form the fractional crystallization of a first mixture of .alpha. and .beta.-zeranol, said mother liquor containing a second mixture of .alpha. the .beta.-zeranol from about 30 to about 70% by weight of the .alpha.-zeranol, the improvement which comprises:
- (i) dehydrogenating said second mixture in the presence of Raney nickel in an n-butyl acetate medium at about reflux temperature and at atmospheric pressure, said dehydrogenation being terminated at about 70 to 90% by weight conversion to produce as a dehydrogenation reaction product a solution, in n-butyl acetate, of zeralanone, and a mixture of .alpha. and .beta.-zeranol;
- (ii) cooling said solution to a temperature of from about 50.degree. C. to about 60.degree. C. under conditions such that said zeralanone and said mixture of .alpha. and .beta.-zeranol do not precipitate;
- (iii) removing said Raney nickel catalyst by filtration from the solution to provide a filtrate comprising an n-butyl acetate solution of zeralanone and of a mixture of .alpha. and .beta.-zeranol;
- (iv) cooling said filtrate, after concentration, to a temperature of from about 10.degree. C. to about 20.degree. C. to precipitate said zeralanone and said mixture of .alpha. and .beta.-zeranol.
Dependencies are inferred from the claim text.