反应详情

To a solution of methyl 6-((4-fluorobenzylamino)methyl)picolinate (140 mg, 0.51 mmol) in THF (3 mL) were added 3,5-dichloro-2-hydroxybenzene-1-sulfonyl chloride (147 mg, 0.56 mmol) and TEA (0.142 mL, 1.02 mmol). The reaction mixture was stirred at rt overnight and concentrated in vacuo. The residue was purified by preparative HPLC. Fractions containing the desired product were combined, concentrated and lyophilized to give the desired product (0.19 g, 74%) as a white solid. 1H NMR (CD3OD) δ 7.93-7.80 (m, 2H), 7.65-7.53 (m, 3H), 7.27-7.25 (m, 2H), 6.94-6.90 (m, 2H), 4.68 (s, 2H), 4.65 (s, 2H), 3.98 (s, 3H). MS (ESI): 499.0 (M+H)+.

1. concentrationconcentrated in vacuo
2. customThe residue was purified by preparative HPLC
3. additionFractions containing the desired product
4. concentrationconcentrated