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 N-(3,5-dimethylpyridin-2-yl)-4-fluoro-N-isobutylbenzenesulfonamide (53.7 mg, 0.160 mmol) and (tetrahydro-2H-pyran-4-yl)methanol (18.54 mg, 0.160 mmol) in dimethyl sulfoxide (DMSO) (1 mL) stirred at room temperature, was added sodium hydride (4.79 mg, 0.160 mmol, 60% wt in mineral oil). The reaction mixture was stirred at 20° C. for 2 hour, then left to stand overnight. Additional sodium hydride (4.79 mg, 0.160 mmol, 60% wt in mineral oil) was added and the reaction stirred for a further 2 hours. The reaction was quenched with methanol (0.5 mL) and water (0.5 mL), then concentrated in vacuo. The crude was purified by mass directed autoprep (formic acid modifier) to give the title compound (31.3 mg). LCMS (2 min, formic) Rt 1.38 min, m/z (ES+) 433 (M+H).
WORKUP
后处理
- waitleft
- waitto stand overnight
- stirringthe reaction stirred for a further 2 hours
- customThe reaction was quenched with methanol (0.5 mL) and water (0.5 mL)
- concentrationconcentrated in vacuo
- customThe crude was purified by mass