反应详情

To a solution of: N-{[2-(2,3-dihydro-4H-1,4-benzothiazin-4-yl)pyridine-3-yl]methyl}-N-pyridin-3-ylpyridin-3-amine (52 mg, 0.126 mmol) in methanol (1.5 mL) and water (1 mL) was added Oxone™ (97 mg, 0.157 mmol). The reaction progress was monitored by LC/MS and after 2 hours the reaction was diluted with water and Na2CO3 solution and the product was extracted into ethyl acetate, the solution dried, filtered, and the solvent evaporated. The residue was purified by chromatography on silica gel eluting with a 20-100% acetone/hexane gradient to give the title compound as a coloress glass. 1H-NMR (500 MHz, CDCl3): δ 8.51 (1H, d, J=3.6 Hz), 8.29 (2H, s), 8.26 (2H, d, J=3.9 Hz), 7.88 (2H, t, J=9.0 Hz), 7.26-7.31 (4H, m), 7.18-7.21 (2H, m), 7.00 (1H, t, J=7.3 Hz), 6.22 (1H, d, J=8.3 Hz), 4.76 (2H, s), 4.38 (2H, br s), 3.57 (2H, t, J=5.8 Hz). m/e (m+1): 444.2.

1. extractionthe product was extracted into ethyl acetate
2. customthe solution dried
3. filtrationfiltered
4. customthe solvent evaporated
5. customThe residue was purified by chromatography on silica gel eluting with a 20-100% acetone/hexane gradient