HRID1269607

反应详情

EQUATION

反应方程式

HRID 1269607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(2-methoxyethyl)-N-[4′-(trifluoromethyl)-1,1′-biphenyl-3-yl]amine (0.1 g, 0.34 mmol) in anhydrous acetonitrile (10 mL) was added ethyl [4-(bromomethyl)-2-methylphenoxy]acetate (0.097 g, 0.34 mmol) and N,N-diisopropylethylamine (0.059 mL, 0.34 mmol). The resulting mixture was heated to reflux and stirred under nitrogen for 3 h. The reaction mixture was concentrated in vacuo and the residue partitioned between water (20 mL) and CH2Cl2 (40 mL), the organic extract was separated by hydrophobic frit and the solvents removed in vacuo. Purification by Biotage™ chromatography (Silica, 12 g) eluting 9:1 cyclohexane:EtOAc afforded the title compound as a colourless oil (90 mg).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. customthe residue partitioned between water (20 mL) and CH2Cl2 (40 mL)
  5. extractionthe organic extract
  6. customwas separated by hydrophobic frit
  7. customthe solvents removed in vacuo
  8. customPurification by Biotage™ chromatography (Silica, 12 g)
  9. washeluting 9:1 cyclohexane