HRID1075314

反应详情

EQUATION

反应方程式

HRID 1075314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

The crude 3-chloro-2-(1-ethoxyethoxy)-1-propyl acetate produced in Example 9 was added over a period of 1.5 hours to a stirred hot (105°) solution of 1.1 kg (27.5 moles) of sodium hydroxide in 1.1 L of water in a 5 L three-necked round-bottomed flask equipped with a mechanical stirrer, a reflux condenser, a dropping funnel, and a thermometer. The mixture was refluxed for an additional 4 hours period and then was allowed to cool to 25° C. The mixture was stirred with 1.5 L of water to dissolve inorganic salts and the phases were separated. The aqueous solution was extracted with 2 L of methylene chloride. Solvent was removed from the methylene chloride layer and the residual oil was combined with the above organic phase to give 1.2 kg of crude 3-(1-ethoxyethoxy) oxetane.

WORKUP

后处理

  1. customequipped with a mechanical stirrer, a reflux condenser, a dropping funnel
  2. temperatureThe mixture was refluxed for an additional 4 hours period
  3. dissolutionto dissolve inorganic salts
  4. customthe phases were separated
  5. extractionThe aqueous solution was extracted with 2 L of methylene chloride
  6. customSolvent was removed from the methylene chloride layer