HRID742996

反应详情

EQUATION

反应方程式

HRID 742996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 5-ethynyl-2-hydroxybenzoate (8 g, 45.4 mmol), prepared according to Example 1 b, was dissolved in a mixture of diethyl ether and light petroleum (200+200 ml) in a hydrogenation flask. Quinoline (1.7 ml) and palladium on CaCO3, poisoned with Pb (Lindlax catalyst; 200 mg) were added, and the flask was attached to an atmospheric pressure hydrogenation apparatus. The mixture was stirred for 2 h at room temperature, by then the calculated amount of hydrogen had been consumed. The catalyst was filtered off and the solution was evaporated to dryness. The product was purified by flash column chromatograpy on silica, using toluene as an eluent. A nearly quantitative yield was obtained.

WORKUP

后处理

  1. additionwere added
  2. customby then the calculated amount of hydrogen had been consumed
  3. filtrationThe catalyst was filtered off
  4. customthe solution was evaporated to dryness
  5. customThe product was purified by flash column chromatograpy on silica
  6. customA nearly quantitative yield was obtained