HRID2182019

反应详情

EQUATION

反应方程式

HRID 2182019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Into another flask, KOH (25.8 g), HO(CH2)5OH (47.9 g) and dioxane (200 ml) were charged and stirred at 90° C. until KOH was dissolved. Then, from a dropping funnel, PhCH2OCH2CH(CH3)OTs (71.2 g) and dioxane (75 ml) were added at 90° C. over a period of 20 minutes. After further stirring at 80° C. for 20 hours, water (350 ml) was added. Extraction with dichloromethane (100 ml) was carried out three times, and the extracted organic phase was washed with water (150 ml), then dried over anhydrous magnesium sulfate, filtered and further concentrated. The concentrated liquid was purified by silica gel column (eluent: hexane/ethyl acetate) to obtain PhCH2OCH2CH(CH3)O(CH2)5OH(20.8 g).

WORKUP

后处理

  1. dissolutionwas dissolved
  2. extractionExtraction with dichloromethane (100 ml)
  3. washthe extracted organic phase was washed with water (150 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationfurther concentrated
  7. customThe concentrated liquid was purified by silica gel column (eluent: hexane/ethyl acetate)