FIELD: chemistry.
SUBSTANCE: invention relates to a method for the preparation of 3-O-sulfamate 16,16-dimethyl-D-homoequilenine of formula (1), in which the keto group 16,16-dimethyl-3-methoxy-D-homoestra-1,3,5 (10),8,14-pentaen-17a-one is protected with a dioxolane group by the reaction of ethylene glycol and p-toluenesulfonic acid to give 16,16-dimethyl-3-methoxy-D-homoestra-1,3,5(10),8,14-pentaene-17a- [1,3-dioxalane], after which the stage of aromatization is carried out under the action of Raney Nickel, deprotection and methoxy group 16,16-dimethyl-3-methoxy-D-homoestra-1,3,5(10),6,8-pentaene-17a-[1,3-dioxalane] is carried out simultaneously by boiling in a mixture of acetic and hydrobromic acids, sulfamolichloride is added to a solution of 16,16-dimethyl-D-homoequilenine, purified by recrystallization, and the target product (1) is obtained.
EFFECT: new method for obtaining 3-O-sulfamate 16,16-dimethyl-D-homoequilenine of formula (1) in high yield has been developed, in which stages with hazardous reagents and solvents are excluded and in which intermediate products are used without additional purification.
(1)
1 cl, 2 ex
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