HRID1197624

反应详情

EQUATION

反应方程式

HRID 1197624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe mixture was quenched with NH4Cl
  2. extractionextracted three times with ethyl acetate
  3. washwashed with sat. NaCl
  4. dry with materialdried (MgSO4)
  5. filtrationAfter filtering
  6. customthe solvent was evaporated