HRID1762781

反应详情

EQUATION

反应方程式

HRID 1762781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 100.0 grams of triethanolamine and 58 milliliters of dry pyridine in 350 milliliters of dry dichloromethane was stirred at room temperature under a nitrogen atmosphere. A solution of 8.0 grams of (4-chloroformyl-9-fluorenylidene)malononitrile in 400 milliliters of dry dichloromethane was added over a period of 1 hour. After addition, the reaction mixture was further stirred for another hour. The reaction mixture was washed several times with water to remove the excess amines and the corresponding hydrochloride salts, dried with anhydrous magnesium sulfate and filtered. Evaporation of the filtrate gave 5 grams of crude product. Purification by recrystallization from isopropanol afforded 4.5 grams of pure (1c), mp., 155.5°-156.5° C.

WORKUP

后处理

  1. additionAfter addition
  2. washThe reaction mixture was washed several times with water
  3. customto remove the excess amines
  4. dry with materialthe corresponding hydrochloride salts, dried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customEvaporation of the filtrate
  7. customgave 5 grams of crude product
  8. customPurification
  9. customby recrystallization from isopropanol