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ChemicalBook CAS DataBase List Hydroxyprogesterone caproate
630-56-8

Hydroxyprogesterone caproate synthesis

5synthesis methods
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Yield:630-56-8 19.8 g

Reaction Conditions:

Stage #1:17-hydroxyprogesterone;hexanoic acid with pyridine;toluene-4-sulfonic acid in toluene at 110 - 120; for 3 h;
Stage #2: with hydrogenchloride in ethanol;water for 2 h;Reflux;Reagent/catalyst;Solvent;

Steps:

1
17α- hydroxy progesterone 20g, n-hexanoic acid 40ml, pyridine 16ml, p-toluenesulfonic acid 1.6g, toluene300ml, into 500ml three-necked flask, the reaction temperature was raised to between 110 ~ 120°C 3 hours. sampling The reaction was monitored by TLC. The reaction is as follows 17α- hydroxyprogesterone concentration treatment made after completion of the reaction,concentration treatment method for a concentrated under reduced pressureToluene, pyridine and n-hexanoic acid. After concentration in a three-neck flask was added the end of 100ml of ethanol, in 3 ml of concentrated hydrochloric acid, heated under reflux, alcohol solution for 2 hours. Sampling the reaction was monitored by TLC, complete hydrolysis of the diester into progesterone caproate after the reaction was stopped. The reaction is as follows: n-caproic acid was cooled to below 5 ° C, filtration, drying in progesterone caproate crude 24g, crude yield 120%. Progesterone caproate crude product was purified with ethanol to give progesterone caproate boutique 19. 8g, progesterone caproate Collectibles The yield progesterone caproate crude 82.5%, the total yield of 99.0%.

References:

Jiangsu Grand Xinyi Pharmaceutical Co.,Ltd.;KONG, LEI CN104017041, 2016, B Location in patent:Paragraph 0013-0015; 0017-0019

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