HRID494600

反应详情

EQUATION

反应方程式

HRID 494600 的结构方程式

PROCEDURE

实验过程

2-Phenylbutyric acid (10 g, 61 mmole) was dissolved in methanol (30 ml) treated with concentrated HCl (1 ml) and heated at reflux for 20 hours. The heating was stopped and the reaction mixture cooled to room temperature. The solvent was removed in vacuo and the oily residue was treated with ethyl acetate (100 ml). The organic layer was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a clear oil. Yield 10.61 g (97%). 1H NMR (300 MHz, DMSO-d6): δ ppm 0.81 (t, J=7.35 Hz, 3H) 1.69 (m, 1H) 1.98 (m, 1H) 3.53 (d, J=7.35 Hz, 1H) 3.58 (s, 3H) 7.30 (m, 5H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 20 hours
  3. customThe solvent was removed in vacuo
  4. additionthe oily residue was treated with ethyl acetate (100 ml)
  5. washThe organic layer was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo