HRID329998

反应详情

EQUATION

反应方程式

HRID 329998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To sodium salt of 2-hydroxynaphthalene-6-carboxylic acid methyl ester (44.8 g) N,N-dimethylformamide (200 ml) was added with stirring at room temperature. Then a solution of m-xylylenedichloride (17.5 g, 0.1 mol) in N,N-dimethylformamide was added in drops thereto in 10 minutes. The reaction mixture was stirred at 105° C. for 4 hours and then cooled to give a precipitate. The precipitate was rinsed with N,N-dimethylformamide, treated with hot water at 80° C. for 30 minutes with stirring, and then with methanol at 60° C. for 30 minutes with stirring; cooled, filtered and dried to give a white crystals of 1,3-bis(6-carbomethoxy-2-naphthoxymethyl)benzene (39.7 g, yield 77.8%): m.p. 177.3°-178.0° C.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 105° C. for 4 hours
  2. temperaturecooled
  3. customto give a precipitate
  4. washThe precipitate was rinsed with N,N-dimethylformamide
  5. additiontreated with hot water at 80° C. for 30 minutes
  6. stirringwith stirring
  7. stirringwith methanol at 60° C. for 30 minutes with stirring
  8. temperaturecooled
  9. filtrationfiltered
  10. customdried