HRID1601089

反应详情

EQUATION

反应方程式

HRID 1601089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NBS (8.43 g, 47.4 mmol) and AIBN (2.1 g, 12.8 mmol) were added to a solution of 1-BOC-2-methylbenzimidazole (10.0 g, 43.1 mmol) in CCl4 (120 mL) at reflux. After 21 h, the reaction was cooled and filtered. The filtrate was concentrated, and the resulting brown oil was chromatographed (silica gel, 15% EtOAc/hexanes) to afford the title compound: 1H NMR (400 MHz, CDCl3) δ 7.94-8.01 (m, 1 H), 7.70-7.75 (m, 1 H), 7.31-7.44 (m, 2 H), 4.96 (s, 2 H), 1.75 (s, 9 H),

WORKUP

后处理

  1. temperatureat reflux
  2. temperaturethe reaction was cooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. customthe resulting brown oil was chromatographed (silica gel, 15% EtOAc/hexanes)