反应详情

To a solution of [4-amino-2-(piperidin-4-ylamino)-pyrimidin-5-yl]-(5-fluoro-2-methoxy-phenyl)-methanone trifluoroacetic acid salt (0.0589 mmol, Example 22) in methylene chloride (1.25 mL) were added triethylamine (0.065 mL, 0.466 mmol, Aldrich) and a solution of ethanesulfonyl chloride (8.1 mg, 0.062 mmol, Aldrich 99+%) in methylene chloride (0.33 mL) at 0° C. After 5 minutes the reaction mixture was allowed to stir at room temperature for 1 hr before it was concentrated in vacuo. The residue was absorbed on silica gel and purified with 99.5/0.5495/5 of methylene chloride/methanol to give [2-amino-6-(1-ethanesulfonyl-piperidin-4-ylamino)-pyridin-3-yl]-(5-fluoro-2-methoxy-phenyl)-methanone as a white solid (16.0 mg, 63% yield). HRMS, observed: 437.1660, Calcd for (M+H)+: 437.1654.

1. customat 0° C
2. concentrationwas concentrated in vacuo
3. customThe residue was absorbed on silica gel
4. custompurified with 99.5/0.5495/5 of methylene chloride/methanol