HRID2279046

反应详情

EQUATION

反应方程式

HRID 2279046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 0° C. solution of 1-(benzyloxy)-2-chloro-3-fluoro-4-nitrobenzene (45 g, 160 mmol) in DCM (200 mL) was treated drop-wise with tribromoborane (7.9 g, 320 mmol) over 0.5 h, stirred at 0° C. for 2 h, treated with satd. NaHCO3 and was washed with brine. The organic layer was dried over Na2SO4 and concentrated to afford 2-chloro-3-fluoro-4-nitrophenol (25 g, 82%). 1H NMR (400 MHz, DMSO-d6): δ 9.39 (s, 1 H), 6.95 (m, 2 H), 4.67 (brs, 2H).

WORKUP

后处理

  1. additiontreated with satd
  2. washNaHCO3 and was washed with brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated