HRID1076906

反应详情

EQUATION

反应方程式

HRID 1076906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthen filtered
  2. customThe filtrate was evaporated to dryness
  3. customleaving a residue which
  4. filtrationfiltered
  5. extractionextracted with methylene chloride
  6. additiontreated with ethereal HCl
  7. filtrationThe resulting precipitate was filtered
  8. customrecrystallized from methanol-diethyl ether and hydrated in a constant humidity chamber