HRID1506747

反应详情

EQUATION

反应方程式

HRID 1506747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 6,9-dichloro-2-methoxyacridine (100 mg, 0.36 mmol) and phenol (approximately 1.5 g) was heated to 100° C. under nitrogen atmosphere and stirred for 1 hour. 1-Ethylpiperidin-4-amine (92 mg, 0.72 mmol) was added to the mixture. The reaction was stirred at 100° C. for 5 hours, cooled to 20-25° C., and diluted with dichloromethane. The mixture was washed twice with sodium hydroxide solution (1 N) and twice with ammonium chloride solution. The phases were separated, and the organic layer was dried and concentrated. The residue was purified by Biotage column chromatography using triethylamine (5%) and methanol (5 to 15%) in dichloromethane to give the title compound; MS (Found: M+1=370).

WORKUP

后处理

  1. stirringThe reaction was stirred at 100° C. for 5 hours
  2. temperaturecooled to 20-25° C.
  3. washThe mixture was washed twice with sodium hydroxide solution (1 N) and twice with ammonium chloride solution
  4. customThe phases were separated
  5. customthe organic layer was dried
  6. concentrationconcentrated
  7. customThe residue was purified by Biotage column chromatography