HRID1818769

反应详情

EQUATION

反应方程式

HRID 1818769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture was stirred for 16 hours
  2. customThe mixture was quenched with saturated NH4Cl
  3. additiondiluted with ether
  4. washThe mixture was washed with water, brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe crude product was purified via Isco chromatography (Redisep, silica, gradient 5-30% ethyl acetate in hexane)