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
A mixture of 6-bromo-2-methyl-3-nitropyridine (100 g, 461 mmol) and sodium methanesulfinate (47.0 g, 461 mmol) in DMSO (300 mL) was stirred at room temperature for 1.5 h. The reaction mixture was poured into ice-water (1 L) and stirred until all the ice had melted. The ice-cold solution was filtered, and a dark purple solid was collected. The solid collected was dissolved in ethyl acetate (1 L). The solution was treated with activated charcoal, filtered through Celite™. The Celite™ cake was washed with ethyl acetate, and the filtrate was collected. The solvent was evaporated from the filtrate under reduced pressure to give the title compound (87.0 g, 87%) as a yellow solid. Exact mass calculated for C7H8N2O4S: 216.0. Found: LCMS m/z=217.2 (M+H+).
WORKUP
后处理
- filtrationThe ice-cold solution was filtered
- customa dark purple solid was collected
- customThe solid collected
- dissolutionwas dissolved in ethyl acetate (1 L)
- additionThe solution was treated with activated charcoal
- filtrationfiltered through Celite™
- washThe Celite™ cake was washed with ethyl acetate
- customthe filtrate was collected
- customThe solvent was evaporated from the filtrate under reduced pressure