HRID594127
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
- 70 °C
PROCEDURE
实验过程
To a solution of pyridine (0.083 mL, 1.023 mmol) and 3,5-dimethyl-2-pyridinamine (125 mg, 1.023 mmol) in dichloromethane (1 mL) was added 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (309 mg, 1.023 mmol). The mixture was heated at 70° C. for 4 hours. Water (5 mL) was added and the organic phase separated and purified by flash silica (Si) chromatography (50% dichloromethane-ethyl acetate gradient) to give the title compound (56 mg) as a bright yellow solid. LCMS (2 min, formic) Rt 0.93 min, m/z (ES+) 388 (M+H).
WORKUP
后处理
- customthe organic phase separated
- custompurified by flash silica (Si) chromatography (50% dichloromethane-ethyl acetate gradient)