135270-11-0 synthesis

Yield:135270-11-0 97%

Reaction Conditions:

with calcium hydride;4-methylenepiperidine monohydrochloride in acetonitrile at 80 - 85; for 20 h;Reagent/catalyst;

Steps:

1-15

Put 3.77g (0.09mol) calcium hydride, 11.97g (0.09mol) 4-methylenepiperidine hydrochloride, 60mL acetonitrile into a 100mL there-necked flask, stir at room temperature for 30min, drop into 15g (0.06mol) (2R,3S)-2-(2,4-difluorophenyl)-3-methyl-[(1H-1,2,4-triazol-1-yl)methyl]oxirane, stir and heat up to 80-85 , and react for 20h. After the reaction, concentrated, extracted with ethyl acetate, crystallized with ethanol and water, and dried to obtain 20.2 g of white solid fluconazole with a yield of 97% and a purity of 99.98%.

References:

CN113929660,2022,A Location in patent:Paragraph 0045-0096