HRID1174915

反应详情

EQUATION

反应方程式

HRID 1174915 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 2-amino-4-nitrophenol (15.8 g, 102 mmol) and potassium xanthate (18.2 g, 114 mmol) in pyridine (200 mL). Reflux for 1 hour and then cool to room temperature. Pour the reaction into concentrated HCl (100 mL) and ice. Filter and wash the product with 1 N HCl to remove excess pyridine. Dry in a vacuum oven at 50° C. for 48 h to afford the title compound (15.9 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

  1. temperatureReflux for 1 hour
  2. additionPour
  3. filtrationFilter
  4. washwash the product with 1 N HCl
  5. customto remove excess pyridine
  6. customDry in a vacuum oven at 50° C. for 48 h