HRID2103077
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturerefluxed for 3 hours
- filtrationThe reaction mixture was filtered
- concentrationconcentrated
- dissolutionThe organic residue was dissolved in warm hexane
- customto crystallize out in the fridge
- filtrationAfter filtration, 2-methoxy-1,3-dimethyl-5-nitrobenzene
- customwas collected as white solid (12 g)