HRID555203

反应详情

EQUATION

反应方程式

HRID 555203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 100 g of 2,2-adamantane dimethanol, 48.2 g of methacrylic acid, 20 g of toluene, 25 g of acidic ion-exchange resin Amberlist-15, and 0.1 g of 2,2′-methylenebis(6-t-butyl-p-cresol) was heated at 120° C. for 6 hours while the water being formed was azeotroped off. After the reaction mixture resumed room temperature, it was filtered through Celite. The filtrate was concentrated in vacuum. 300 g of hexane was added to the concentrate for recrystallization. The crystals were recovered and dried in vacuum, obtaining 45.0 g (yield 33%) of the target compound. The spectral data of this compound were identical with those of the product in Synthesis Example 1-2.

WORKUP

后处理

  1. customformed
  2. customwas azeotroped off
  3. customresumed room temperature
  4. filtrationit was filtered through Celite
  5. concentrationThe filtrate was concentrated in vacuum
  6. addition300 g of hexane was added to the
  7. concentrationconcentrate for recrystallization
  8. customThe crystals were recovered
  9. customdried in vacuum