HRID249249
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
To N-(3-fluoro-4-pyridinyl)-N-(3-methyl-1H-indol-1-yl)glycine ethyl ester (5.0 g) in 100 ml of tetrahydrofuran cooled to ice bath temperature was added lithium aluminum hydride (1M solution in tetrahydrofuran, 30 ml) via syringe. The reaction was stirred for 0.5 hour. The mixture was quenched with NH4Cl and extracted three times with ethyl acetate. The organics were combined, washed with sat. NaCl and dried (MgSO4). After filtering, the solvent was evaporated to yield a solid (3.9 g) which was eluted with 50% ethyl acetate/dichloromethane on a silica gel column via high pressure liquid chromatography (HPLC). The desired fractions were evaporated to yield 3.7 g of a solid, m.p. 123°-125° C.
WORKUP
后处理
- customThe mixture was quenched with NH4Cl
- extractionextracted three times with ethyl acetate
- washwashed with sat. NaCl
- dry with materialdried (MgSO4)
- filtrationAfter filtering
- customthe solvent was evaporated