HRID1818769
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
2-Fluoroaniline (1.45 mL, 15 mmol) was dissolved in DMF (10 mL) and sodium hydride (0.58 g, 15 mmol) was added and the mixture was stirred for 30 minutes. 2-Fluoronitrobenzene (1.05 mL, 10 mmol) was added and the mixture was stirred for 16 hours. The mixture was quenched with saturated NH4Cl and diluted with ether. The mixture was washed with water, brine, dried over anhydrous magnesium sulfate, and concentrated. The crude product was purified via Isco chromatography (Redisep, silica, gradient 5-30% ethyl acetate in hexane) to afford 1.4 g 2-fluoro-N-(2-nitrophenyl)aniline that was carried on directly to the next step. MS (ES) m/z 232.9.
WORKUP
后处理
- stirringthe mixture was stirred for 16 hours
- customThe mixture was quenched with saturated NH4Cl
- additiondiluted with ether
- washThe mixture was washed with water, brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe crude product was purified via Isco chromatography (Redisep, silica, gradient 5-30% ethyl acetate in hexane)