HRID655068

反应详情

EQUATION

反应方程式

HRID 655068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 193.7 g 3-[5-methyl-2-(tetrahydro-pyran-2-yloxy)-phenyl]-acrylic acid ethyl ester (Bunce, R., Moore, J., Org. Prep. Proc., 29(3), 293 (1997)) and 2 g p-toluenesulfonic acid in 2.5 l of ethanol was stirred at room temperature for 24 hours. Then the reaction mixture was concentrated and the residue was diluted with ether, washed with saturated sodium bicarbonate and brine, dried and evaporated to dryness. The resulting yellow solid was recrystallized to yield 97.7 g of colourless crystals.

WORKUP

后处理

  1. concentrationThen the reaction mixture was concentrated
  2. additionthe residue was diluted with ether
  3. washwashed with saturated sodium bicarbonate and brine
  4. customdried
  5. customevaporated to dryness
  6. customThe resulting yellow solid was recrystallized