HRID625262

反应详情

EQUATION

反应方程式

HRID 625262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a −78° solution of 110 mg of 2-(2-nitro-5-(piperidin-1-yl)phenyl)isonicotinaldehyde in 4 mL of THF was added 0.82 mL of a 1.0 M solution of 3-(trifluoromethyl)phenylmagnesium chloride in THF. After 5 min the solution was warmed to 0° C. and treated with 10 mL of a saturated aqueous solution of NaHCO3. The mixture was extracted with ethyl acetate and the organic extracts were washed with water and then with brine. The solution was dried (Na2SO4) and the solvent was evaporated. The residue was purified by silica gel chromatography eluting with 1:1 ethyl acetate/hexanes to give 123 mg of product. MS (ES, m/z) 458.2 [M+H]+.

WORKUP

后处理

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic extracts were washed with water
  3. dry with materialThe solution was dried (Na2SO4)
  4. customthe solvent was evaporated
  5. customThe residue was purified by silica gel chromatography
  6. washeluting with 1:1 ethyl acetate/hexanes