HRID1077395

反应详情

EQUATION

反应方程式

HRID 1077395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6.1 g of 4-(6-methacryloyloxyhexyloxy)benzoic acid were converted to the acid chloride in a manner similar to example 6. This substance was taken up in 100 ml of tetrahydrofuran (THF) and added dropwise at 0° to 5° C. to a stirred solution of 3.3 g of hydroquinone monobutyl ether in 100 ml of THF and 4 ml of triethylamine. The mixture was stirred for a further 3 hours at room temperature and the triethylamine hydrochloride was then filtered out. The filtrate was evaporated to dryness and the residue dissolved in 50 ml of dichloromethane. The solution was washed several times with water, dried with sodium sulphate and the solvent then distilled off. The crude product so obtained was purified by column chromatography and recrystallisation from n-hexane.

WORKUP

后处理

  1. filtrationthe triethylamine hydrochloride was then filtered out
  2. customThe filtrate was evaporated to dryness
  3. dissolutionthe residue dissolved in 50 ml of dichloromethane
  4. washThe solution was washed several times with water
  5. dry with materialdried with sodium sulphate
  6. distillationthe solvent then distilled off