HRID2119080

反应详情

EQUATION

反应方程式

HRID 2119080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 374 mg of ethyl 3,3-dimethyl-4-pentenoate, 400 mg of 3-phenoxybenzyl alcohol and 16 mg of sodium ethoxide in 10 ml of toluene was heated under reflux for 24 hours, with a Dean-Stark apparatus containing a molecular sieve to absorb the evolved ethanol. The mixture was neutralized by adding an anhydrous ether solution of hydrogen chloride. The neutral solution was poured into water. The ether layer was separated, dried over magnesium sulfate, and distilled to give 520 mg (70% yield) of 3-phenoxybenzyl 3,3-dimethyl-4-pentenoate, b.p. 155°-158°/0.3 mm.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours, with a Dean-Stark apparatus
  3. additioncontaining a molecular sieve
  4. customto absorb the evolved ethanol
  5. additionby adding an anhydrous ether solution of hydrogen chloride
  6. additionThe neutral solution was poured into water
  7. customThe ether layer was separated
  8. dry with materialdried over magnesium sulfate
  9. distillationdistilled