HRID1972402
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
A 250 ml, round-bottomed flask was charged with lithium aluminum hydride (1.871 g, 49.3 mmol) and THF (75 mL). After cooling to 0° C., 3-(benzyloxymethyl)piperazine-2,5-dione (3.85 g, 16.44 mmol) was slowly added. The mixture was warmed to room temperature and then heated at reflux for 1 h. After this time, the mixture was cooled to 0° C. and the reaction was quenched with sodium sulfate decahydrate (20 g) and stirred vigorously for 1 h. The mixture was filtered, and the filtrate was concentrated to give 2-(benzyloxymethyl)piperazine (2.60 g) as a yellow oil. This material was taken to the next step without purification.
WORKUP
后处理
- temperatureThe mixture was warmed to room temperature
- temperatureheated
- temperatureat reflux for 1 h
- temperatureAfter this time, the mixture was cooled to 0° C.
- customthe reaction was quenched with sodium sulfate decahydrate (20 g)
- filtrationThe mixture was filtered
- concentrationthe filtrate was concentrated