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    • 5. 发明专利
    • AT308980B
    • 1973-07-25
    • AT394571
    • 1971-05-06
    • RICHTER GEDEON VEGYESZET
    • TUBA ZOLTAN DRBOR MARIAKOMESZ ZOLTANWEITNER EVAGOEROEG SANDOR DR
    • C07J31/00C07J43/00C07C167/34
    • 1306622 21 - (4 - Methyl - 1 - piperazinyl)- Steroid RICHTER GEDEON VEGYESZETI GYAR RT 30 April 1971 [13 May 1970] 12350/71 Heading C2U [Also in Division A5] In the preparation of 11#,17α-dihydroxy-21- (4 - methyl - 1 - piperazinyl) - pregna - 1,4-. diene - 3,20 - dione from prednisolone 21- methanesulphonate and N-methylpiperazine, the reaction is effected in an acetonitrilebenzene mixture of 60 : 40 to 40 : 60 v/v composition, preferably in the presence of an alkali metal halide and/or alkaline earth metal halide, whereby an easily filterable product is obtained which may, if desired, be converted into a mono- or di-salt thereof with an acid, e.g. hydrochloric. Further quantities of product obtainable by evaporating the mother liquor are purified by conversion to the dihydrochloride which is then either reacted with the free base to yield the monohydrochloride or is reacted with aqueous alkali metal hydroxide to yield the free base. The following compounds are said to be byproducts of the above process and/or prior art processes. (a) 11 #, 17α, 21,21 -tetrahydroxypregna- 1,4 -diene- 3,20 - dione; (b) 3 - oxo - 11#,17α,20- trihydroxypregna - 1,4 - dien - 21 - oic acid; (c) 3 - oxo - 11#,17α - dihydroxy - 21 - pyridiniopregna - 1,4,20 - trien - 20 - olate; and (d) 3 - oxo - 11#,20 - dihydroxypregna - 1,4,17(20)- trien-21-ol. Prednisolone 21-methanesulphonate is prepared from prednisolone by reaction with mesyl chloride. Reference has been directed by the Comptroller to Specification 954,146.