HRID1951396

反应详情

EQUATION

反应方程式

HRID 1951396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.10 g (4.84 mmol) of 4-(2-acetyl-3-oxobut-1-en-1-yl)-3-methylbenzonitrile are taken up in 30 ml of isopropanol and, after addition of 592 mg (4.84 mmol) of 4-aminopyridin-2(1H)-one, heated at the reflux temperature for 72 h. The mixture is then concentrated, and the residue is again taken up in isopropanol and filtered through silica gel with isopropanol as eluent. The residue after concentration of the filtrate is mixed with a little methanol and crystallized. The precipitated product is filtered off, washed with diethyl ether and dried under high vacuum. 348 mg (22.5% of theory) of the title compound are obtained.

WORKUP

后处理

  1. temperatureheated at the reflux temperature for 72 h
  2. concentrationThe mixture is then concentrated
  3. filtrationfiltered through silica gel with isopropanol as eluent
  4. additionThe residue after concentration of the filtrate is mixed with a little methanol
  5. customcrystallized
  6. filtrationThe precipitated product is filtered off
  7. washwashed with diethyl ether
  8. customdried under high vacuum