HRID1814765

反应详情

EQUATION

反应方程式

HRID 1814765 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-methoxy-6-methyl-2-nitropyridine (S. Lindstrom, T. Ahmad and S. Grivas, Heterocycles (1994), 38(3), 529-540) (30 mmole) and N-bromosuccinimide (60 mmole) in CCl4 (50 ml) was refluxed under a 500 watt tungsten lamp for 16 hours, cooled, filtered and evaporated. A portion (2.4 g) of the crude product was mixed with sodium formate (1 g), water (1 ml) and ethanol (7 ml), refluxed for 24 hours, cooled and concentrated to low volume. The residue was partitioned between dichloromethane and water, the organic dried and evaporated. Chromatography gave the title compound (25%).

WORKUP

后处理

  1. temperaturecooled
  2. filtrationfiltered
  3. customevaporated
  4. additionA portion (2.4 g) of the crude product was mixed with sodium formate (1 g), water (1 ml) and ethanol (7 ml)
  5. temperaturerefluxed for 24 hours
  6. temperaturecooled
  7. concentrationconcentrated to low volume
  8. customThe residue was partitioned between dichloromethane and water
  9. customthe organic dried
  10. customevaporated