HRID1076908

反应详情

EQUATION

反应方程式

HRID 1076908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 41.9 g (0.1 mole) of 2,7-bis(5-chlorovaleryl)-xanthene, 2 g of potassium iodide, 100 ml of diallylamine and 200 ml. of tetrahydrofuran was heated and stirred at 120°C. for 24 hours. After cooling, the reaction mixture was filtered and the filtrate evaporated to dryness. The resulting residue was cooled, dissolved in 10% HCl, extracted with diethyl ether and made alkaline. The product was extracted with methylene chloride, evaporated to dryness, recrystallized six times from heptane and dried in vacuo to give the desired product. M.P. 54°-55°C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. customthe filtrate evaporated to dryness
  4. temperatureThe resulting residue was cooled
  5. dissolutiondissolved in 10% HCl
  6. extractionextracted with diethyl ether
  7. extractionThe product was extracted with methylene chloride
  8. customevaporated to dryness
  9. customrecrystallized six times from heptane
  10. customdried in vacuo