反应详情

温度

0 °C

Methanesulfonyl chloride (59 mg, 0.52 mmol) was added to a mixture of 2-(2-(4-fluoro-benzyl)-5-(5-chloro-2-(methylthio)pyrimidin-4-yl)thiophen-3-yl)ethanol (170 mg, 0.43 mmol) and diisopropylethylamine (72 mg, 0.55 mmol) in dichloromethane (8 mL) at 0° C. After stirring at 0° C. for 1 h, the solvent was removed in vacuo. Acetonitrile (5 mL) and morpholine (112 mg, 1.29 mmol) were added to the residue and the mixture was heated to 70° C. overnight. After cooling to rt solvent was evaporated in vacuo and the product was purified by flash chromatography eluting with methanol (1 M ammonia)/dichloromethane (1:20) to afford the title compound (148 mg, 74%). MS (M+H)+ 464/466.

1. customthe solvent was removed in vacuo
2. temperaturethe mixture was heated to 70° C. overnight
3. temperatureAfter cooling to rt solvent
4. customwas evaporated in vacuo
5. customthe product was purified by flash chromatography
6. washeluting with methanol (1 M ammonia)/dichloromethane (1:20)