HRID595915

反应详情

EQUATION

反应方程式

HRID 595915 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a steel bomb, (+/−)-4-(6-fluoropyridin-3-yl)-1-methylpiperidin-2-one (341 mg, 1.638 mmol) was added followed by addition of ammonium hydroxide solution (0.00 mmol)—remaining 40% head space. The reactor was heat at 150° C. for 20 hr (internal pressure built up to 100 psi upon heating). After cooling down, the reaction was completed. The whole solvent (transferred to a flask) was removed in vacuo. Toluene was added and co-evaporated to remove water. The crude product, (+/−)-4-(6-aminopyridin-3-yl)-1-methylpiperidin-2-one, was used for the next step without further purification (87%). LCMS (m/z): 206.1 (MH+), 0.24 min.

WORKUP

后处理

  1. temperature(internal pressure built up to 100 psi upon heating)
  2. temperatureAfter cooling down
  3. customThe whole solvent (transferred to a flask) was removed in vacuo
  4. additionToluene was added
  5. customto remove water
  6. customThe crude product, (+/−)-4-(6-aminopyridin-3-yl)-1-methylpiperidin-2-one, was used for the next step without further purification (87%)
  7. custom206.1 (MH+), 0.24 min.