HRID639632

反应详情

EQUATION

反应方程式

HRID 639632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed
  2. customthe gum was partitioned in water/ethyl acetate
  3. customThe organic layer was isolated
  4. dry with materialdried over MgSO4
  5. customthe solvent was removed in vacuo
  6. custompurified by column chromatography on silica eluting with a gradient of 1% to 5% of methanol in ethyl acetate