HRID35685

反应详情

EQUATION

反应方程式

HRID 35685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Cyclopropanecarbonyl chloride (1.5 ml) was addded dropwise to a mixture of N,N-dimethylaniline (2.4 ml), 4-dimethylaminopyridine (5.0 mg) and 8-chloro-4,5-dihydro-1-methyl-1H -pyrazolo[4,3-c]quinoline (2.0 g) in chloroform (20 ml) at 0° C. and the mixture was allowed to stir at that temperature for 2 hours. After the solvent was evaporated in vacuo, the residue was mixed with 5% hydrochloric acid and extracted with ethyl acetate. The extract was washed with 5% hydrochloric acid, saturated aqueous sodium hydrogen carbonate and water and then dried over magnesium sulfate. The solvent was evaported in vacuo to give light brown powder (2. 0 g), which was recrystallized from a mixture of n-hexane and ethyl acetate to afford 8-chloro-5-cyclopropylcarbonyl-4,5-dihydro-1-methyl-1H-pyrazolo[4,3-c]quinoline as colourless prisms.

WORKUP

后处理

  1. customAfter the solvent was evaporated in vacuo
  2. additionthe residue was mixed with 5% hydrochloric acid
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with 5% hydrochloric acid, saturated aqueous sodium hydrogen carbonate and water
  5. dry with materialdried over magnesium sulfate
  6. customto give light brown powder (2. 0 g), which
  7. customwas recrystallized from a mixture of n-hexane and ethyl acetate