HRID1042985

反应详情

EQUATION

反应方程式

HRID 1042985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-3-nitro-4-quinolinamine (see Intermediate 19, 2.4 g, 5.77 mmol) in a mixture of ethanol (60 ml) and THF (20 ml), was added SnCl2,2H2O (7.81 g, 34.6 mmol). The reaction mixture was refluxed for 3 h and then concentrated to dryness. The resulting residue was poured into aqueous sodium hydroxide. The organic phase was extracted with EtOAc, washed with water, dried and concentrated to give the title compound as a yellow solid (2 g, 71%). [APCI-MS] m/z: 387 MH+, Rt 3.37 min.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 3 h
  2. concentrationconcentrated to dryness
  3. additionThe resulting residue was poured into aqueous sodium hydroxide
  4. extractionThe organic phase was extracted with EtOAc
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated