HRID594168
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a solution of (tetrahydro-2H-pyran-4-yl)methanol (20.08 mg, 0.173 mmol) and 4-fluoro-N-(5-isopropylpyridin-2-yl)-N-(oxetan-3-ylmethyl)benzenesulfonamide (63 mg, 0.173 mmol) in dimethyl sulfoxide (DMSO) (1 mL) stirred in air at room temperature was added sodium hydride (6.91 mg, 0.173 mmol, 60% wt in mineral oil). The reaction mixture was stirred at 20° C. for 2 hours. The reaction mixture was carefully quenched with methanol (2 mL) and water (2 mL), then solvents evaporated in vacuo. The crude product was purified by flash silica (Si) (25% ethyl acetate-cyclohexane gradient) to give the title product (63.2 mg). LCMS (2 min, High pH) Rt 1.23 min, m/z (ES+) 461 (M+H).
WORKUP
后处理
- customThe reaction mixture was carefully quenched with methanol (2 mL) and water (2 mL)
- customsolvents evaporated in vacuo
- customThe crude product was purified by flash silica (Si) (25% ethyl acetate-cyclohexane gradient)