HRID2355939
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
- 60 °C
PROCEDURE
实验过程
(1-Benzyl-piperidin-4-yl)-(2-nitro-benzyl)-amine (0.25 g, 0.7 mmol) and zinc dust (0.2 g, excess) were combined in 75% aqueous acetic acid (8 mL) and stirred at 60° C. for 2 h. After cooling to room temperature, the solvents were removed in vacuo and the resultant crude mixture dissolved in water (10 mL), followed by addition of ammonium hydroxide until pH 3 was attained. The solution was extracted with methylene chloride (3×). The organic layers were pooled together, washed with water (2×), brine (2×), dried over sodium sulfate, filtered, and concentrated to afford 0.18 g (79%) of the desired product.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe solvents were removed in vacuo
- dissolutionthe resultant crude mixture dissolved in water (10 mL)
- additionfollowed by addition of ammonium hydroxide until pH 3
- extractionThe solution was extracted with methylene chloride (3×)
- washwashed with water (2×), brine (2×)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated