HRID1643697

反应详情

EQUATION

反应方程式

HRID 1643697 的结构方程式

PROCEDURE

实验过程

To a solution of 3,5-bis-methoxymethoxy-4-((E)-3-phenyl-allyl)-benzoic acid (220g) (18 g, 0.05 mol) in MeOH (300 mL) was added catalytic amount of conc. H2SO4 (3 mL) in one portion. The mixture was refluxed overnight. The solution was concentrated. The residue was dissolved in CH2Cl2 (75 mL) and washed with sat. NaHCO3 (25 mL). The organic layers were dried and concentrated to give a brown solid (12 g, 73% yield). 1H NMR (400 MHz, CDCl3): δ 9.63 (s, 2H), 7.11˜7.34 (m, 5H), 6.93 (s, 2H), 6.32 (s, 2H), 3.77 (s, 3H), 3.42 (s, 2H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed overnight
  2. concentrationThe solution was concentrated
  3. dissolutionThe residue was dissolved in CH2Cl2 (75 mL)
  4. washwashed with sat. NaHCO3 (25 mL)
  5. customThe organic layers were dried
  6. concentrationconcentrated