HRID329996

反应详情

EQUATION

反应方程式

HRID 329996 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 p-hydroxybenzoic acid benzyl ester (45.6 g, 0.2 mol) in 200 ml N,N-dimethylformamide, sodium carbonate (10.6 g, 0.1 mol) was added and stirred for 10 minutes at room temperature. Then a solution of m-xylylenedichloride (17.3 g, 0.1 mol) in 100 ml of N,N-dimethylformamide was added in drops to the reaction mixture in 10 minutes. The reaction mixture stirred at 113° C. for 4 hours, cooled and blown into water, and the obtained precipitate was filtered, rinsed with water. Then crued product was suspended in methanol and stirred at 60° C. for 30 minutes, cooled, filtered, and gave 15.8 g (yield 26.9%) of 1,3-bis(p-carbobenzyloxyphenoxymethyl)-benzene: m.p. 92.5°-93.8° C.

WORKUP

后处理

  1. stirringThe reaction mixture stirred at 113° C. for 4 hours
  2. temperaturecooled
  3. filtrationthe obtained precipitate was filtered
  4. washrinsed with water
  5. stirringstirred at 60° C. for 30 minutes
  6. temperaturecooled
  7. filtrationfiltered