HRID1720273

反应详情

EQUATION

反应方程式

HRID 1720273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 150 mg (0.78 mmol) of 4-chloro-2-methylquinolin-6-ol, 174 mg (0.81 mmol) of n-tetradecylamine, and 5 mL of n-butanol was heated under reflux for 24 hours. Excess butanol was removed by codistillation with cyclohexane. The residue was chromatographed on 30 g of silica gel (eluent 1:9 methanol-dichloromethane) to furnish crude product. This was taken up in methanol, and the solution was treated with dry hydrogen chloride gas. The solution was evaporated under reduced pressure to give the title compound as crystalline material: m.p. 180°-183° C.

WORKUP

后处理

  1. temperatureunder reflux for 24 hours
  2. customExcess butanol was removed by codistillation with cyclohexane
  3. customThe residue was chromatographed on 30 g of silica gel (eluent 1:9 methanol-dichloromethane)
  4. customto furnish crude product
  5. customThe solution was evaporated under reduced pressure