HRID594125

反应详情

EQUATION

反应方程式

HRID 594125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-((3,5-dimethylisoxazol-4-yl)methoxy)benzene-1-sulfonyl chloride (241 mg, 0.800 mmol) in pyridine (5 mL), stirred under nitrogen at room temperature, was added 5-isopropylpyridin-2-amine (54.5 mg, 0.4 mmol). The mixture was then stirred at room temperature overnight. Dichloromethane (25 mL) was added to the mixture and the organic phase washed with water (25 mL) and brine (25 mL) then dried using a hydrophobic frit. Solvent was removed in vacuo to give the crude product. This was purified by flash silica (Si) chromatography (0-100% ethyl acetate-cyclohexane gradient), to provide the title compound (39 mg) as an off-white solid. LCMS (2 min, formic) Rt 0.96 min, m/z (ES+) 402 (M+H).

WORKUP

后处理

  1. washthe organic phase washed with water (25 mL) and brine (25 mL)
  2. customthen dried
  3. customSolvent was removed in vacuo
  4. customto give the crude product
  5. customThis was purified by flash silica (Si) chromatography (0-100% ethyl acetate-cyclohexane gradient)