HRID1880759

反应详情

EQUATION

反应方程式

HRID 1880759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 60 ml of tetrahydrofuran were added 4.98 ml of trifluoromethyltrimethylsilane and 3 g of isonicotinealdehyde, and 0.09 g of tetrabutylammonium fluoride trihydrate was added at 0° C., and the mixture was stirred for 1 hour. Thereafter, 10% hydrochloric acid was added at 0° C., and the mixture was stirred for 3 hours, and poured into an aqueous saturated sodium bicarbonate solution. After extraction with ethyl acetate three times, the organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 4.7 g of 2,2,2-trifluoro-1-pyridin-4-yl-ethanol.

WORKUP

后处理

  1. additionwas added at 0° C.
  2. stirringthe mixture was stirred for 3 hours
  3. extractionAfter extraction with ethyl acetate three times
  4. washwashed with an aqueous saturated sodium chloride solution
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated