HRID641806

反应详情

EQUATION

反应方程式

HRID 641806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-methyl-6-nitroquinoline (12 g, 63.84 mmol) in HCl (1N, 450 mL) was added a solution of SnCl2.2H2O (72 g, 0.32 mol) in HCl (1N, 150 mL) slowly. The reaction mixture was heated to reflux for 15 min, then cooled to room temperature. The precipitate was filtered. The filtrate was basified by aqueous KOH and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure to give 6.9 g of 2-methylquinolin-6-amine (68.3%). MS [M++1]=159, LC-MS: tR=0.255 min.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 15 min
  3. filtrationThe precipitate was filtered
  4. extractionextracted with EtOAc
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. customthe solvent was removed under reduced pressure