HRID2287048

反应详情

EQUATION

反应方程式

HRID 2287048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,2-Dimethyl-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1-[2-(tetrahydro-2-pyranyloxy)ethylidene]-1,2,3,4-tetrahydronaphthalene (151 g), dissolved in 1100 ml of dioxan is submitted to a catalytic hydrogenation at atmospheric pressure and roomtemperature, the catalyst being 10 g of 5% palladium on charcoal. After some 80 percent of the calculated amount of hydrogen has been consumed, the hydrogen uptake tends to slow down and an additional quantity of 2 g of catalyst is needed to bring the reduction to an end. The catalyst is removed by filtration and the filtrate is evaporated in vacuo. The residue does not tend to crystallize. It contains a mixture of two stereoisomers of the title product and it is applied without purification in the next synthesis.

WORKUP

后处理

  1. customAfter some 80 percent of the calculated amount of hydrogen has been consumed
  2. customThe catalyst is removed by filtration
  3. customthe filtrate is evaporated in vacuo
  4. customto crystallize
  5. additiona mixture of two stereoisomers of the title product and it
  6. customis applied without purification in the next synthesis