1179-87-9Relevant articles and documents
Preparation method of algestone acetophenide
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Paragraph 0026; 0033; 0038; 0043; 0048; 0053; 0054; 0055, (2017/07/21)
The invention discloses a preparation method of algestone acetophenide. The preparation method comprises the following steps: (1) performing reaction among androstenedione cyanohydrin ketal, 1 to 1.5 times amount of substance of phosphorus oxychloride and 1 to 10 times amount of substance of an alkaline medium for 1 to 5h at the reaction temperature of -10 to 80 DEG C to obtain a suppressor; (2) performing reaction between the suppressor and 1 to 10 times amount of substance of methyl magnesium chloride for 1 to 5h at the reaction temperature of -10 to 70 DEG C to obtain a Grignard's product; (3) performing reaction between the Grignard's product and 1 to 5 times amount of substance of potassium permanganate for 10 to 60m at the reaction temperature of -10 to 30 DEG C, and then performing reaction between the Grignard's product and 1 to 5 times amount of substance of acid for 1 to 10h at the reaction temperature of -10 to 30 DEG C to obtain a hydroxy compound; (5) performing reaction among the hydroxy compound, 0.025 to 0.1 time amount of substance of a catalyst and 2 to 10 times amount of substance of acetyl benzene for 1 to 10h at the reaction temperature of -10 to30 DEG C to obtain the algestone acetophenide. Not only the quality and yield of a product are improved, but also the production cost is reduced and the process time is shortened.
