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ChemicalBook CAS DataBase List (22R,23R)-2A,3A,22,23-TETRAHYDROXY-24-ETHYL-BETA-HOMO-7-OXA-5A-CHOLESTAN-6-ONE

(22R,23R)-2A,3A,22,23-TETRAHYDROXY-24-ETHYL-BETA-HOMO-7-OXA-5A-CHOLESTAN-6-ONE synthesis

2synthesis methods
-

Yield:82373-95-3 95%

Reaction Conditions:

with sodium hypochlorite in water at 25; for 0.5 h;Ionic liquid;Baeyer-Villiger Ketone Oxidation;Reagent/catalyst;Temperature;

Steps:

1-5

Successively add intermediate b (392.1g), [MIM-CH2CHClCOOH]2HPW12O40 (78.3g), water (784ml) to the reactor. Add sodium hypochlorite (95.5g) under stirring at 25 ° C. The reaction is held for 0.5h. Using equal volumes of saturated sodium thiosulfate solution wash three times, extracted with ethyl acetate, and centrifuged to recover [MIM-CH2CHClCOOH]2HPW12O40, washed with saturated brine, and dried to obtain 28-homobrassinolide (400.5 g, purity 96.1%, yield 95.0%).

References:

CN110452284,2019,A Location in patent:Paragraph 0012-0013; 0024; 0026-0027; 0029-0030; 0036; 0038