HRID1703347

反应详情

EQUATION

反应方程式

HRID 1703347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.5 g of 2-[bis-(phenoxy)methyl]-6-(phenoxy)pyridine in 15 ml of 1,4-dioxane was added dropwise, 5 percent sulfuric acid until the mixture just became turbid. The mixture was heated over a steam bath at 80°-90° C. for about 10 minutes. The reaction mixture was poured into 20 ml of water, producing a yellowish emulsion and then extracted with 50 ml of ethyl ether. The extract was washed with 50 ml of a 5 percent aqueous sodium hydroxide solution and thrice with 50 ml portions of water and then with 50 ml of a saturated sodium chloride solution. The extract was then dried over sodium sulfate and the solvent removed by evaporation under reduced pressure. The residue was a yellow-orange oil which solidified partially on cooling to yield 0.3 g of the desired product. The product was confirmed by Infrared and Nuclear Magnetic resonance analysis.

WORKUP

后处理

  1. temperatureThe mixture was heated over a steam bath at 80°-90° C. for about 10 minutes
  2. customproducing a yellowish emulsion
  3. extractionextracted with 50 ml of ethyl ether
  4. washThe extract was washed with 50 ml of a 5 percent aqueous sodium hydroxide solution and thrice with 50 ml portions of water
  5. dry with materialThe extract was then dried over sodium sulfate
  6. customthe solvent removed by evaporation under reduced pressure
  7. temperatureon cooling