HRID1750472

反应详情

EQUATION

反应方程式

HRID 1750472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (0.117 g, 3.08 mmol) was added to a solution of 2-{[4-(trifluoromethyl)pyridin-2-yl]methyl}cyclopentan-1-one (0.375 g, 1.54 mmol) in ethanol (10 ml). The reaction was stirred at room temperature for 3 hours and then quenched with water (5 mL) and 2M HCl (aq., 5 ml). The organics were extracted with ethyl acetate (2×30 ml) and the combined organics were washed with brine (10 ml), dried over magnesium sulfate, filtered through a hydrophobic frit and concentrated in vacuo. The crude product was purified by column chromatography (silica, 0-35% ethyl acetate/petrol) to afford the title compound as two diastereomers.

WORKUP

后处理

  1. customquenched with water (5 mL) and 2M HCl (aq., 5 ml)
  2. extractionThe organics were extracted with ethyl acetate (2×30 ml)
  3. washthe combined organics were washed with brine (10 ml)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through a hydrophobic frit
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by column chromatography (silica, 0-35% ethyl acetate/petrol)