Preparation method of pediatric asthma drug budesonide
A compound and solvent technology, applied in the field of drug preparation, can solve the problems of long synthesis route, low overall reaction yield, uneconomical and reasonable overall route, etc., and achieves convenient and simple post-processing, high enantioselectivity, Split effect ideal effect
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Embodiment 1
[0028] step 1):
[0029] In a 10L three-necked flask, add 3L of 1-butyl-3-methylimidazolium bisulfate ([BMIM]HSO 4 ) and 2L of dichloromethane, 40g (0.56mol) of n-butyraldehyde and 208g (0.5mol) of compound I were added, and the reaction was stirred at 30°C for 10h, and the reaction was monitored by TLC until the reaction was complete. The reaction solution was directly concentrated under reduced pressure until no liquid flowed out, and a large amount of white solid was precipitated, which was suction filtered. The filtrate is mainly ionic liquid, which can be recycled directly. The filter cake was rinsed with dichloromethane (200ml) to obtain 231.9g (98.7% yield) of a white solid, and the ratio of its isomers R and S was 85:15.
[0030] Step (2):
[0031] Add 150 g (0.32 mol) of compound II, 5 L of absolute ethanol and 1 L of dichloromethane into a 10 L three-neck flask, stir and dissolve at room temperature. Add 160g (+)-camphorsulfonic acid (0.69mol), heat to 50°C, the ...
Embodiment 2
[0037] step 1):
[0038] In a 10L three-necked flask, add 6L of N-ethylpyridine bisulfate ([EPy]HSO 4 ) and 1L of dichloromethane, added 40g (0.56mol) of n-butyraldehyde and 208g (0.5mol) of compound I, stirred and reacted at 30°C for 5h, and monitored the reaction by TLC until the reaction was complete. The reaction solution was directly concentrated under reduced pressure until no liquid flowed out, and a large amount of white solid was precipitated, which was suction filtered. The filtrate is mainly ionic liquid, which can be recycled directly. The filter cake was rinsed with dichloromethane (200ml) to obtain 223.7g (95.2% yield) of a white solid, and the ratio of isomers R and S was 87:13.
[0039] Step (2):
[0040] Add 150 g (0.32 mol) of compound II, 5 L of absolute ethanol and 1 L of dichloromethane into a 10 L three-neck flask, stir and dissolve at room temperature. Add 120g (+)-tartaric acid (0.8mol), heat to 40°C, the solid disappears completely, and keep the re...
Embodiment 3
[0046] step 1):
[0047] In a 10L three-necked flask, add 3L tetraethylammonium bisulfate ([TEAm]HSO 4 ) and 2L of dichloromethane, 40g (0.56mol) of n-butyraldehyde and 208g (0.5mol) of compound I were added, and the reaction was stirred at 50°C for 4h, and the reaction was monitored by TLC until the reaction was complete. The reaction solution was directly concentrated under reduced pressure until no liquid flowed out, and a large amount of white solid was precipitated, which was suction filtered. The filtrate is mainly ionic liquid, which can be recycled directly. The filter cake was rinsed with dichloromethane (400ml) to obtain 227.7g (96.9% yield) of a white solid, and the ratio of isomers R and S was 89:11.
[0048] Step (2):
[0049] Add 150 g (0.32 mol) of compound II, 5 L of absolute ethanol and 1 L of chloroform into a 10 L three-neck flask, stir and dissolve at room temperature. Add 160g (+)-camphorsulfonic acid (0.69mol), heat to 40°C, the solid disappears compl...
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