HRID639632
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
- 80 °C
PROCEDURE
实验过程
(3-amino-2-benzylamino-6-trifluormethyl-pyridin-4-yl)-carbamic acid ethyl ester (88 mg, 0.25 mmol) was dissolved in 5 mL of acetic acid and the reaction mixture was stirred at 80° C. overnight. The solvent was removed and the gum was partitioned in water/ethyl acetate. The organic layer was isolated, dried over MgSO4, the solvent was removed in vacuo and purified by column chromatography on silica eluting with a gradient of 1% to 5% of methanol in ethyl acetate to give 37 mg of the title compound as a colourless gum.
WORKUP
后处理
- customThe solvent was removed
- customthe gum was partitioned in water/ethyl acetate
- customThe organic layer was isolated
- dry with materialdried over MgSO4
- customthe solvent was removed in vacuo
- custompurified by column chromatography on silica eluting with a gradient of 1% to 5% of methanol in ethyl acetate