HRID601545
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
Combine 2-amino-4-nitrophenol (15.8 g, 102 mmol) and potassium ethyl xanthate (18.3 g, 114 mmol) in pyridine (200 mL). Heat the reaction at reflux for 1 h. Allow the reaction to cool to room temperature and pour into concentrated HCl (100 mL) and ice. Filter and wash the solids with 1N HCl to remove excess pyridine. Dry the solids under house vacuum at 50° C. for 2 days to obtain the title compound (15.85 g, 79%). 1H NMR (400 MHz, DMSO-d6): δ 8.18 (dd, 1H, J=8.8, 2.2 Hz), 7.93 (d, 1H, J=2.2 Hz), 7.73 (d, 1H, J=8.8 Hz).
WORKUP
后处理
- temperatureHeat
- customthe reaction
- temperatureat reflux for 1 h
- customthe reaction
- filtrationFilter
- washwash the solids with 1N HCl
- customto remove excess pyridine
- customDry the solids under house vacuum at 50° C. for 2 days