HRID1493591

反应详情

EQUATION

反应方程式

HRID 1493591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-(4-methoxyphenyl)piperazine dihydrochloride (5.30 g, 20 mmole), 2-chloro-5-nitropyridine (3.2 g, 20 mmole) and potassium carbonate (4.14 g, 30 mmole) in DMF (20 ml) was heated at 120° for 66 hours. The reaction mixture was cooled, diluted with water and the resulting precipitate collected by filtration. To this solid was added methanol (200 ml) and the mixture was heated under reflux for 0.17 hour. After cooling, the solid was collected by filtration and dried to yield the desired product, m.p. 165°-6° (4.0 g, 64%), which was used without further purification.

WORKUP

后处理

  1. temperaturewas heated at 120° for 66 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting precipitate collected by filtration
  4. additionTo this solid was added methanol (200 ml)
  5. temperaturethe mixture was heated
  6. temperatureunder reflux for 0.17 hour
  7. temperatureAfter cooling
  8. filtrationthe solid was collected by filtration
  9. customdried