HRID1076906
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
PROCEDURE
实验过程
A mixture of 18.2 g (0.05 mole) of 2,7-bis(3-chloropropionyl)xanthene, 2 g of potassium iodide, 100 ml. of diethylamine and 100 ml. of tetrahydrofuran was allowed to stand for 3 days then filtered. The filtrate was evaporated to dryness leaving a residue which was treated with 10% HCl and filtered. The filtrate was made alkaline, extracted with methylene chloride and treated with ethereal HCl. The resulting precipitate was filtered, recrystallized from methanol-diethyl ether and hydrated in a constant humidity chamber to give the desired product. M.P. 184.5°-185.5°C.
WORKUP
后处理
- filtrationthen filtered
- customThe filtrate was evaporated to dryness
- customleaving a residue which
- filtrationfiltered
- extractionextracted with methylene chloride
- additiontreated with ethereal HCl
- filtrationThe resulting precipitate was filtered
- customrecrystallized from methanol-diethyl ether and hydrated in a constant humidity chamber