HRID401519

反应详情

EQUATION

反应方程式

HRID 401519 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 1-(4-methoxy-phenyl)-cyclopropanecarboxylic acid (50.0 g, 0.26 mol) in MeOH (500 mL) was added toluene-4-sulfonic acid monohydrate (2.5 g, 13 mmol) at room temperature. The reaction mixture was heated at reflux for 20 hours. MeOH was removed by evaporation under vacuum and EtOAc (200 mL) was added. The organic layer was washed with sat. aq. NaHCO3 (100 mL) and brine, dried over anhydrous Na2SO4 and evaporated under vacuum to give 1-(4-methoxy-phenyl)-cyclopropanecarboxylic acid methyl ester (53.5 g, 99%). 1H NMR (CDCl3, 400 MHz) δ 7.25-7.27 (m, 2H), 6.85 (d, J=8.8 Hz, 2H), 3.80 (s, 3H), 3.62 (s, 3H), 1.58 (m, 2H), 1.15 (m, 2H).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 20 hours
  3. customMeOH was removed by evaporation under vacuum and EtOAc (200 mL)
  4. additionwas added
  5. washThe organic layer was washed with sat. aq. NaHCO3 (100 mL) and brine
  6. dry with materialdried over anhydrous Na2SO4
  7. customevaporated under vacuum