HRID1668747

反应详情

EQUATION

反应方程式

HRID 1668747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,5-dibromobenzyl alcohol (2.0 h, 8 mmol) in tetrahydrofuran (80 mL) was cooled to 5° C. and treated with sodium hydride (dispersion in oil 55%; 316 mg, 8 mmol). The mixture was left to warm to room temperature and stirred for 15 min. Ethyliodide (2.35 g, 15 mmol) was added and the mixture stirred for 5 h. For the working-up, the reaction mixture was evaporated, then extracted with a mixture of ethyl acetate and saturated sodium hydrogencarbonate solution. After the aqueous layer was re-extracted twice with ethyl acetate, the organic layers were combined, dried over sodium sulfate, and evaporated under reduced pressure. There were obtained 1.15 g of the title compound (yield: 52%) as a yellow oil in sufficient purity to be engaged in the next step without further purification.

WORKUP

后处理

  1. waitThe mixture was left
  2. stirringthe mixture stirred for 5 h
  3. customthe reaction mixture was evaporated
  4. extractionextracted with a mixture of ethyl acetate and saturated sodium hydrogencarbonate solution
  5. extractionAfter the aqueous layer was re-extracted twice with ethyl acetate
  6. dry with materialdried over sodium sulfate
  7. customevaporated under reduced pressure