HRID1076908
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered
- customthe filtrate evaporated to dryness
- temperatureThe resulting residue was cooled
- dissolutiondissolved in 10% HCl
- extractionextracted with diethyl ether
- extractionThe product was extracted with methylene chloride
- customevaporated to dryness
- customrecrystallized six times from heptane
- customdried in vacuo