HRID661872

反应详情

EQUATION

反应方程式

HRID 661872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-bromo-2-fluoro-3-nitrobenzene (1.10 g, 5.00 mmol) in ethanol-acetic acid-water (2:2:1) (25 mL) was treated with iron powder (1.396 g, 25.0 mmol) and the mixture was heated at reflux for 1 h. The mixture was cooled to rt and filtered through a Celite pad. The filtrate was concentrated and the residue was partitioned between EtOAc and NaHCO3 (aq). The organic phase was washed with brine, dried and concentrated to provide 3-bromo-2-fluoroaniline as a brown oil (880 mg, 93%). 1H NMR (400 MHz, chloroform-d) δ 6.85-6.92 (1H, m), 6.80 (1H, td, J=8.0, 1.2 Hz), 6.66-6.73 (1H, m), 3.81 (2H, br. s.).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 h
  3. filtrationfiltered through a Celite pad
  4. concentrationThe filtrate was concentrated
  5. customthe residue was partitioned between EtOAc and NaHCO3 (aq)
  6. washThe organic phase was washed with brine
  7. customdried
  8. concentrationconcentrated