HRID2305069

反应详情

EQUATION

反应方程式

HRID 2305069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 4.12 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(5-(2-propenyloxy)pentyloxy)benzene, 0.36 g of mercury (II) sulfate, 5 ml of 1% aqueous sulfuric acid solution, and 50 ml of tetrahydrofuran was stirred at 60° C. for 1 hour. The reaction mixture was filtered through Celite, and the filtrate was poured into diluted hydrochloric acid, and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with diluted hydrochloric acid and water in this order, dried over magnesium sulfate, and concentrated to give a crude product. This crude product was subjected to silica gel chromatography, which afforded 4.05 g (yield, 94%) of 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetone, nD25.5 1.5350.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Celite
  2. additionthe filtrate was poured into diluted hydrochloric acid
  3. extractionextracted twice with diethyl ether
  4. washwashed with diluted hydrochloric acid and water in this order
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customto give a crude product