Preparation method of tibolone intermediate etherate and tibolone

• Main Authors: SUN XIAOMING, LIU XIRONG, JIN ZHIZHONG, ZENG CHUNLING
• Format: Patent
• Language: Chinese; English
• Published: 29.04.2022
• Subjects: CHEMISTRY; METALLURGY; ORGANIC CHEMISTRY; STEROIDS

The invention relates to a preparation method of tibolone intermediate etherate and tibolone, which comprises the following steps: in the presence of a compound shown as a formula (II), ethylene glycol and a compound shown as a formula (I) are subjected to a ketalation reaction, so that ethylene glycol can be selectively subjected to the ketalation reaction with a 3-carbonyl group of the compound shown as the formula (I), and 5 and 10 double bonds are constructed at the same time to obtain a compound shown as a formula (III); and further performing first hydrolysis reaction and etherification reaction on the compound in the formula (III) by a one-pot method to obtain a high-purity compound tibolone intermediate etherate in a formula (IV). The tibolone can be obtained by carrying out alkynylation reaction and hydrolysis reaction on the compound shown in the formula (IV), a new synthesis route is provided for preparing the tibolone, and the method has the advantages of fewer steps, mild reaction conditions and