HRID77854
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
PROCEDURE
实验过程
To a solution of 5-trimethylsilanylethynyl-pyridin-2-ylamine (26 mg, 137 mmol) described in Manufacturing Example 28-1-2 in tetrahydrofuran (1 mL) and methanol (1 mL) was added potassium carbonate (37.9 mg, 274 mmol) at room temperature, which was stirred for 1 hour at room temperature. The reaction solution was partitioned into water and ethyl acetate at 0° C. The organic layer was washed with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1) to obtain the title compound (16 mg, 99%).
WORKUP
后处理
- customThe reaction solution was partitioned into water and ethyl acetate at 0° C
- washThe organic layer was washed with saturated aqueous sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- concentrationthe solvent was concentrated under a reduced pressure
- customThe residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1)