反应详情

温度

50 °C

In a glass pressure vessel, a solution of N-[(4aR,7aR)-6-(5-fluoropyrimidin-2-yl)-7a-(2-thienyl)-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide (6 g, 13.6 mmol) in ethanol (240 mL) is treated with pyridine (11 mL). O-methylhydroxylamine hydrochloride (11.4 g, 136.5 mmol) is added and the mixture is heated at 50° C. for 4 hours. The solution is concentrated and diluted with 1 M hydrochloric acid and ethyl acetate. The aqueous layer is separated and neutralized with 50% w/w aqueous solution of sodium hydroxide to adjust the pH to 9. The white precipitate is filtered and dried under vacuum. The crude product is crystallized in hot methyl-t-butyl ether until a complete solution is formed then the solution is cooled to room temperature. The solid precipitate is filtered and dried under vacuum to give the title compound (3.5 g, 76%). ES/MS (m/e): 336 (M+H).

1. concentrationThe solution is concentrated
2. additiondiluted with 1 M hydrochloric acid and ethyl acetate
3. customThe aqueous layer is separated
4. filtrationThe white precipitate is filtered
5. customdried under vacuum
6. customThe crude product is crystallized in hot methyl-t-butyl ether until a complete solution
7. customis formed
8. temperaturethe solution is cooled to room temperature
9. filtrationThe solid precipitate is filtered
10. customdried under vacuum