HRID1353605

反应详情

EQUATION

反应方程式

HRID 1353605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Into a flame dried flask, N-(1-benzyl-piperidin-4-yl)-2-methoxy-6-nitrobenzamide (1.0 g, 2.8 mmol) and lithium aluminium hydride (0.31 g, 8.45 mmol) were combined. To the mixture was added anhydrous 1,4-dioxane (15 mL). The mixture was slowly brought to reflux over 1 h and stirred at reflux for 16 h. The reaction mixture was cooled to 0° C. and excess lithium aluminium hydride destroyed by dropwise addition of methanol, followed by careful addition of 20% potassium hydroxide. The aluminum salts were filtered, the filtrate concentrated and used as is for the next reaction.

WORKUP

后处理

  1. customInto a flame dried flask
  2. temperatureto reflux over 1 h
  3. temperatureat reflux for 16 h
  4. customexcess lithium aluminium hydride destroyed by dropwise addition of methanol
  5. additionfollowed by careful addition of 20% potassium hydroxide
  6. filtrationThe aluminum salts were filtered
  7. concentrationthe filtrate concentrated
  8. customas is for the next reaction