反应详情

温度

-78 °C

(Diethylamino)sulphur trifluoride (0.337 mL, 2.55 mmol) was added to DCM (13 mL), cooled to −78° C. and treated dropwise with a solution of 1-(6-chloro-4-pyrimidinyl)ethanol (Intermediate 20, 328 mg, 2.068 mmol) in DCM (4 mL) under argon. The resulting mixture was allowed to warm to room temperature and stirred for 4 hours. The reaction was quenched by adding water (5 mL) and extracted with DCM (×2). The DCM layers were separated, combined, dried under magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (Biotage SP4) eluting with a gradient of 0-25% ethyl acetate and iso-hexane. Product containing fractions were combined and evaporated under reduced pressure to give the title compound as a colourless oil (125 mg);

1. temperatureto warm to room temperature
2. customThe reaction was quenched
3. additionby adding water (5 mL)
4. extractionextracted with DCM (×2)
5. customThe DCM layers were separated
6. customdried under magnesium sulfate
7. customevaporated under reduced pressure
8. customThe residue was purified by column chromatography (Biotage SP4)
9. washeluting with a gradient of 0-25% ethyl acetate and iso-hexane
10. additionProduct containing fractions
11. customevaporated under reduced pressure