Synthesis method of budesonide impurity EP-ZG
A technology of EP-ZG and synthesis method, which is applied in the field of drug impurity synthesis to achieve the effects of high yield, good selectivity and simple process route
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Embodiment 1
[0018]
[0019] Take a 1000mL three-neck flask, add 3.01g of budesonide and 900mL of ethanol, stir to dissolve; then add 1.10g of triphenylphosphine rhodium chloride, the system changes from colorless and clear to reddish brown, and hydrogen gas is introduced into the solution and replaced three times. Carry out the reaction at room temperature until the liquid phase detection shows that there is no residue of the raw material budesonide; then directly filter the system, concentrate and dry the filtrate to obtain a black oil, and separate the black oil by column chromatography to obtain 2.7g of gray-brown foamy solid ; The obtained gray-brown foamy solid was slurried with 20ml of acetonitrile for 1 hour, and suction filtered to obtain 1.14g of off-white solid, which was the impurity EP-ZG, with a yield of 37.70% and a purity of 95%.
Embodiment 2
[0021]
[0022] Take a 500mL three-necked flask, add 1.2g of budesonide and 240mL of isopropanol, stir to dissolve; then add 0.24g of triphenylphosphine rhodium chloride, the system changes from colorless and clear to reddish brown, and hydrogen gas is introduced into the solution to replace Three times, the reaction was carried out at room temperature until the liquid phase detection showed that there was no residue of the raw material budesonide; then the system was directly filtered, the filtrate was concentrated and dried to obtain a black oil, and the black oil was separated by mixing column chromatography to obtain 1.02 g of gray-brown foam The obtained gray-brown foamy solid was slurried with 10 ml of acetonitrile for 1 h, and suction-filtered to obtain 0.47 g of impurity EP-ZG, with a yield of 39.10% and a purity of 93.7%.
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