HRID1835966

反应详情

EQUATION

反应方程式

HRID 1835966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 118 g of 4-methyl-1,4-pentanediol, 173 g of methyl 5-norbornene-2-carboxylate, 1.4 g of sodium methoxide and 400 ml of toluene was heated under reflux for 5 hours while distilling off the methanol which formed during the reaction. The reaction solution was cooled, washed with saturated sodium bicarbonate water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was purified by vacuum distillation, collecting 221 g of 4-hydroxy-4-methylpentyl 5-norbornene-2-carboxylate (yield: 93%). The physical data of this product were in good coincidence with those of Synthesis Example 1.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. distillationwhile distilling off the methanol which
  4. customformed during the reaction
  5. temperatureThe reaction solution was cooled
  6. washwashed with saturated sodium bicarbonate water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated in vacuum
  9. distillationIt was purified by vacuum distillation