434-03-7Relevant articles and documents
A Short and Efficient Synthetic Method for the Corticosteroid Side-Chain from 17-Keto Steroids
Kataoka, Hideaki,Watanabe, Kiyoshi,Miyazaki, Ken-ichi,Tahara, Shin-ichiro,Ogu, Ken-ichi,et al.
, p. 1705 - 1708 (1990)
21-Acyloxy-16(17)-ene-20-keto steroids were synthesized from 17-keto steroids in 4 steps using palladium(II)-catalyzed oxidative rearrangement of propargyl esters as a key reaction.
A method for synthesis of alkyne progesterone
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Paragraph 0025; 0037-0040; 0043-0046, (2017/12/28)
The invention discloses a synthesis method of ethisterone which is prepared by adopting 4AD namely soybean oil tailings as a raw material, carrying out etherification protection as well as two-step reaction, namely, ethynylation and hydrolysis, and then refining. According to the invention, the raw material is replaced, that is the industrial tailing fermentation product 4AD of the soybean oil is used to replace diene; the raw material is wide in supply, low in cost and little in pollution; the reaction route is short; the process is simple; the auxiliary materials are commonly used chemical products; the generation amount of waste gas, waste water and waste solid is small and is a quarter of that generated in the traditional process.
Process for the preparation of danazol
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Paragraph 0013; 0018; 0019; 0037; 0041, (2019/02/04)
The invention discloses preparation methods of danazol and an intermediate thereof. The preparation method of danazol is prepared by the steps of taking androstenedione as a starting raw material, and carrying out 3-site enol etherification, 17-site carbonyl ethinylation, 3-site hydrolysis, 2-site methylidynel hydroxylation and oximation to obtain danazol. The 3-site enol etherification comprises firstly carrying out a reaction of androstenedione and triethyl orthoformate for 4-10 h in the presence of absolute ethyl alcohol and p-toluenesulfonic acid and at the temperature of 30-50 DEG C, then adding triethylamine at the temperature of 0-10 DEG C, and continuing to carry out a reaction for 0.2-1 h; the 17-site carbonyl ethinylation comprises firstly carrying out a reaction of a potassium hydroxide powder for 1-2 h in an acetylene airflow and at the temperature of 5-10 DEG C, and then carrying out a reaction with the 3-site enol etherified product for 2-4 h in the presence of tetrahydrofuran and a catalyst, at the temperature of 15-30 DEG C and in the acetylene airflow. The 3-site enol etherification is mild in reaction conditions and relatively high in yield, and the 17-site carbonyl ethynylation is relatively high in reaction yield and relatively short in time.