HRID985483
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
PROCEDURE
实验过程
A solution of ethyl 2-[6-(methylamino)-2-pyridyl]acetate (2.2 g, 12.5 mmol) in THF (30 ml) was added dropwise to a suspension of lithium aluminum hydride (1.24 g, 31.2 mmol) in TEF (25 ml) under argon at 0° C. The reaction was stirred for 30 minutes and quenched carefully with water (4 ml) and 1 N NaOH (4 ml). The mixture was filtered through a pad of Celite and washed several times with ethyl acetate. The filtrate was dried with sodium sulfate, filtered, and evaporated under vacuum. The crude product was chromatographed over silica gel to yield 1.50 g (79%) of 2-[6-(Methylamino)-2-pyridyl]ethan-1-ol.
WORKUP
后处理
- customquenched carefully with water (4 ml) and 1 N NaOH (4 ml)
- filtrationThe mixture was filtered through a pad of Celite
- washwashed several times with ethyl acetate
- dry with materialThe filtrate was dried with sodium sulfate
- filtrationfiltered
- customevaporated under vacuum
- customThe crude product was chromatographed over silica gel