Method for preparing steroids and novel intermediate compound used therein
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A compound and Chinese-style technology, applied in the field of pine preparation, can solve the problems of long production cycle, reduced yield of final product, and increased impurity content of final product
Inactive Publication Date: 2008-02-06
TIANJIN PHARMA GROUP CORP
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However, the above-mentioned microbial conversion method has a long production cycle, and needs to use chloroform or methanol as an extractant for multiple extractions, resulting in a reduction in the yield of the final product; while the chemical synthesis method of first ring opening and subsequent iodolation will affect the structure of the final product. For example, 20-ketone may be transformed into a hydroxyl group, or the 17 and 20 positions may form a ring, and the impurity content of the final product will increase
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Embodiment 1
[0084] 30ml of methanol and 8 grams of iodine were stirred to make iodine solution for later use. Put 60ml of tetrahydrofuran, 6g of calcium oxide, and 10g of Sml into the reaction flask, stir for 10 minutes, then slowly add iodine solution dropwise at 15-20°C, stir for 3 hours after the addition, dilute in 10% acetic acid / water (V / V) 500ml, after stirring for 1 hour, filter to obtain Sm2. mp: 132-140°C. Its infrared data is as follows:
[0087] Put 60ml of acetone and Sm2 into the reaction flask, stir for 10 minutes, add 8 grams of potassium acetate and heat up to 60-70°C, keep it warm for 4 hours, then reduce to 40°C and concentrate under reduced pressure. Dilute in 500ml of water after a large number of crystals appear, and stir After 1 hour, it was filtered, washed with water until neutral, and dried to obtain 10.53 g of Sm3 solid. mp: 205-209°C. Its infrared data is as follows:
[0090] Add 30ml of 50-55% hydrogen bromide / water (V / V) solution and 30ml of acetic acid into the reaction flask, cool down to 0°C and slowly add 10g of Sm3 under stirring, after the addition, keep warm at 10°C for 3 hours, after the reaction is completed, The reaction solution was diluted in 600ml of water, washed with water until neutral and dried to obtain Sm4 for later use.
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Abstract
The present invention relates to an improved preparation method of glucocorticoids steroid, in particular to the preparation methods of prednisolone acetate, cortisone, prednisolone or hydrocortisone. The present invention also relates to a new intermediate compound used in the process of preparing the compounds. The present invention provides a new synthetic route of iodo first and opening the ring after, improving the selectivity of final products, reducing the impurity content of the products, and satisfying the color scale of glucocorticoids drugs, thereby conquering the disadvantages of preparing 17 alpha- hydroxyl at first, and then preparing 21-hydroxyl or the derivatives during the process of preparing 17 alpha, 21-hydroxyl steroid or the derivatives of prior art.
Description
technical field [0001] The present invention relates to an improved preparation method of steroidal compounds of glucocorticoids, more particularly to a preparation method of prednisone acetate, prednisolone, cortisone or hydrocortisone. The present invention also relates to novel intermediates for the preparation of the above compounds. Background technique [0002] Now there are two main approaches for the preparation of steroid drugs, one is the microbial transformation approach, and the other is the chemical synthesis approach. As for the preparation of 17α, 21-dihydroxy steroids or their derivatives, the traditional synthesis process is to first prepare 17α-hydroxyl, and then prepare 21-hydroxyl or its derivatives. Carrying out the ring-opening reaction with 16,17-epoxide as a raw material first introduces 17α-hydroxyl, and then prepares the approach of 21-hydroxyl is a more commonly used synthetic process. The process of converting the hydrogen at the 21-position into...
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