HRID2103077

反应详情

EQUATION

反应方程式

HRID 2103077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-Dimethyl-4-nitroaniline (15 g) Me2SO4 (22 g) and K2CO3 (23 g) were dissolved in 150 mL acetone and refluxed for 3 hours. The reaction mixture was filtered and concentrated. The organic residue was dissolved in warm hexane and let to crystallize out in the fridge. After filtration, 2-methoxy-1,3-dimethyl-5-nitrobenzene was collected as white solid (12 g). 1H-NMR (300 MHz, CDCl3): δ=7.95 (s, 2H), 3.80 (s, 3H), 2.38 (s, 6H) ppm. MS: m/z 182 (100, M+H)+

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. filtrationThe reaction mixture was filtered
  3. concentrationconcentrated
  4. dissolutionThe organic residue was dissolved in warm hexane
  5. customto crystallize out in the fridge
  6. filtrationAfter filtration, 2-methoxy-1,3-dimethyl-5-nitrobenzene
  7. customwas collected as white solid (12 g)