HRID1095947

反应详情

EQUATION

反应方程式

HRID 1095947 的结构方程式

PROCEDURE

实验过程

2-Chloro-5-methoxy-benzeneacetic acid (10 g, [CAS Reg. No. 91367-10-1]) was dissolved in MeOH (210 mL) and H2SO4 (0.7 mL) was added. The mixture was then refluxed overnight. Methanol was removed in vacuo and the residue was dissolved in ethyl acetate. The organic layer was washed with sat. NaHCO3 and brine, dried over Na2SO4 and evaporated. The title compound was obtained as a light brown oil (10.16 g, 95%) and was used without further purification. 1H-NMR (δ, CDCl3): 7.27 (d, 1H), 6.83 (d, 1H), 6.77 (dd, 1H), 3.79 (s, 3H), 3.74 (s, 2H), 3.72 (s, 3H).

WORKUP

后处理

  1. temperatureThe mixture was then refluxed overnight
  2. customMethanol was removed in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe organic layer was washed with sat. NaHCO3 and brine
  5. dry with materialdried over Na2SO4
  6. customevaporated