HRID1373894

反应详情

EQUATION

反应方程式

HRID 1373894 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 suspension of 2-methyl-1H-imidazo[4,5-c]quinolin-1-amine hydrochloride (1.79 g, 7.62 mmol) in 30 mL of 2,2-dimethoxypropane was treated with 90 mg of p-toluenesulfonic acid. The reaction mixture was heated to 100° C. overnight. The reaction mixture was then treated with 10 mL of H2O and 10 mL of MeOH, and heating was continued for 24 h. The reaction mixture was cooled and concentrated under reduced pressure. The resulting oil was dissolved in 50 mL of CHCl3 and washed with 2% Na2CO3 solution, H2O and brine. The organic portion was dried over Na2SO4, filtered and concentrated to give N-isopropylidene(2-methyl-1H-imidazo[4,5-c]quinolin-1-yl)amine (1.82 g) as a yellow solid.

WORKUP

后处理

  1. temperatureheating
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe resulting oil was dissolved in 50 mL of CHCl3
  5. washwashed with 2% Na2CO3 solution, H2O and brine
  6. dry with materialThe organic portion was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated