HRID1814765
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooled
- filtrationfiltered
- customevaporated
- additionA portion (2.4 g) of the crude product was mixed with sodium formate (1 g), water (1 ml) and ethanol (7 ml)
- temperaturerefluxed for 24 hours
- temperaturecooled
- concentrationconcentrated to low volume
- customThe residue was partitioned between dichloromethane and water
- customthe organic dried
- customevaporated