HRID2223495

反应详情

EQUATION

反应方程式

HRID 2223495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of Lithium Aluminium Hydride (0.68 g) in diethylether (70 mL) was added portionwise 1-cyanomethyl-5-trifluoromethoxy-1H-indole-2-carboxylic acid ethyl ester (2.28 g). The reaction mixture was then stirred for 16 hours at reflux. The solution was then slowly poured into a saturated solution of sodium-potassium tartrate. The mixture was then extracted with ethyl acetate 3 times. The combined organic phases were then washed with brine, dried with magnesium sulfate, concentrated in vacuo and purified by column chromatography to yield the desired compound (0.83 g, 45%).

WORKUP

后处理

  1. temperatureat reflux
  2. extractionThe mixture was then extracted with ethyl acetate 3 times
  3. washThe combined organic phases were then washed with brine
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. custompurified by column chromatography