Synthesis process of vecuronium bromide
A synthesis process and compound technology, which is applied in the direction of drug combination, steroids, anesthetics, etc., can solve the problems of high cost, inconvenient operation, and low yield, and achieve the effects of mild conditions, avoiding cumbersome operations, and high yield
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[0028] 1), the preparation of compound epiandrosterone sulfonyl ester (III):
[0029] Dissolve epiandrosterone (II) (40.0g, 0.1379mol), p-toluenesulfonyl chloride (45.0g, 0.236mol) in pyridine (250ml), react at 40°C for 3h, pour the reaction solution into water (670ml), filter , a white solid was obtained, washed with water (3×20ml), and dried to obtain product (III) (58.6g, 95.7%), mp 163-165°C.
[0030] 2), 5α-androst-2-en-17-one (IV)
[0031] The compound epiandrosterone sulfonyl ester (III) (50.0g, 0.1125mol) was added to 2,4,6-collidine (100ml), heated to reflux for 4h, and the reaction solution was poured into 10% dilute sulfuric acid ( 150ml), a white solid was precipitated, filtered to obtain an off-white solid, washed with water (3×20ml), and dried to obtain product (IV) (24.5g, 80.0%), mp 108-110°C.
[0032] 3), 17-acetoxy-5α-androstane-2,16-diene (V)
[0033] (IV) (15.0g, 0.055mol), p-toluenesulfonic acid (1.5g, 0.009mol) and isopropenyl acetate (50ml) were heate...
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