HRID85325

反应详情

EQUATION

反应方程式

HRID 85325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

In 8 ml of N,N-dimethylformamide, 375 mg (1.84 mmol) of 7,7,8,8-tetracyanoquinodimethane was dissolved. With stirring under ice cooling, 600 mg (1.75 mmol) of dibutyl[3-methoxy-4-[2-(thiophene-2-yl)vinyl]phenyl]amine was dissolved in 2 ml of N,N-dimethylformamide and added dropwise. The mixture was stirred for 1 hour and further stirred with heating at 50° C. overnight. After the reaction mixture was poured into 80 ml of water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate and concentration were performed. The residue was purified by silica gel column chromatography and washed with chloroform to give 132 mg of a yellowish white crystal having a mp of 211-214° C. (yield: 14.5%).

WORKUP

后处理

  1. additionadded dropwise
  2. stirringThe mixture was stirred for 1 hour
  3. stirringfurther stirred
  4. washwashing with a saturated saline solution
  5. dry with materialdrying over anhydrous sodium sulfate and concentration
  6. customThe residue was purified by silica gel column chromatography
  7. washwashed with chloroform