PREMARIN synthesis

Yield: 95.7%

Reaction Conditions:

with pyridine;triethylamine sulfur trioxide at 55 - 60;Reagent/catalyst;Temperature;

Steps:

1.1; 2.1; 3.1 (1) estro-1,3,5 (10) -triene-17-one Sulfate Preparation (P-1)
100.0 g (370.0 mmol) of estro-1,3,5 (10) -triene-17-one was dissolved in 500 ml of pyridine,154.2 g (851.0 mmol) of sulfonation reagent triethylamine triethylamine were added under stirring, and the internal temperature was 55-60 ° C for 2-3 hours. After completion of the reaction, it was concentrated in vacuo to obtain a crude product. The concentrate was slurried with 400 ml of methanol at room temperature for 1 h, filtered, washed, and dried under vacuum at 50 ° C. for 8 h to obtain 124.0 g of a white solid with a yield of 95.7% and a purity of 98.5%.

References:

Shanghai Gao Zhun Pharmaceutical Co., Ltd.;Li Weihua;Liu Zhenhao;Ding Yongzhen;Lv Liangfei;Zhu Changbin CN110590896, 2019, A Location in patent:Paragraph 0027-0029; 0033-0035; 0039-0041