HRID2250255
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
- 0 °C
PROCEDURE
实验过程
Into a flame dried flask, N-(1-benzyl-piperidin-4-yl)-2-methoxy-6-nitro-benzamide (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
- customInto a flame dried flask
- temperatureto reflux over 1 h
- temperatureat reflux for 16 h
- customexcess lithium aluminium hydride destroyed by dropwise addition of methanol
- additionfollowed by careful addition of 20% potassium hydroxide
- filtrationThe aluminum salts were filtered
- concentrationthe filtrate concentrated
- customas is for the next reaction