HRID1524196

反应详情

EQUATION

反应方程式

HRID 1524196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(6-Bromo-3-nitro-pyridin-2-yl)-(2-chloro-pyridin-4-yl)amine (step 1) (1 eq, 0.303 mmol, 100 mg) is dissolved in MeOH/THF (6 ml of a 1:1 mixture) and stirred for 5 minutes at RT. Zinc (22 eq, 6.6 mmol 350 mg) is added and the reaction mixture is stirred for a further 20 minutes. Saturated aqueous ammonium chloride (0.8 ml) is added to the reaction mixture and stirring continued at room temperature for 30 minutes. The mixture is filtered through CELITE® and the filtrate is diluted with water (10 ml) and extracted with EtOAc (2×10 ml). The organic portions are combined, dried (MgSO4) and concentrated in vacuo to afford the title compound; [M+H]+300.

WORKUP

后处理

  1. stirringthe reaction mixture is stirred for a further 20 minutes
  2. stirringstirring
  3. waitcontinued at room temperature for 30 minutes
  4. filtrationThe mixture is filtered through CELITE®
  5. additionthe filtrate is diluted with water (10 ml)
  6. extractionextracted with EtOAc (2×10 ml)
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo