HRID333459

反应详情

EQUATION

反应方程式

HRID 333459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NBS (5.45 g, 30.62 mmol) and benzoyl peroxide (75% aq, 200 mg, 0.85 mmol) were added to a solution of 4-iodo-2-nitrotoluene (4.63 g, 17.60 mmol) in CCl4 (60 mL). The mixture was heated to reflux overnight, then cooled to room temperature, concentrated in vacuo, and purified by column chromatography to yield 1-bromomethyl-4-iodo-2-nitrobenzene (2.71 g, 45%). 1H NMR (400 MHz, CDCl3): δ 8.35 (d, 1H, J=1.8 Hz, Ph-H), 7.93 (dd, 1H, J=1.8 and 8.1 Hz, Ph-H), 7.30 (d, 1H, J=8.1 Hz, Ph-H), 4.76 (s, 2H, PhCH2).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux overnight
  3. concentrationconcentrated in vacuo
  4. custompurified by column chromatography