HRID79854

反应详情

EQUATION

反应方程式

HRID 79854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 4,4′-Dibromo-2′-methoxy-biphenyl-2-ylamine (3.5 g, 9.8 mmol) in H2SO4 (2.4 g) and water (8.5 ml) at 0° C. was added slowly a solution of NaNO2 (682 mg, 9.8 mmol) in water (9 ml). The mixture was stirred at 0° C. for 2 hours. Urea (1.2 g, 20 mmol) was added and the mixture was stirred for 12 hours. The mixture was diluted with water and was heated at 70° C. for 24 hours. The mixture was cooled to 25° C. and was filtered. The collected solid was re-crystallized from benzene/methanol to give 3,7-dibromo-dibenzofuran (2.27 g).

WORKUP

后处理

  1. stirringthe mixture was stirred for 12 hours
  2. temperaturewas heated at 70° C. for 24 hours
  3. temperatureThe mixture was cooled to 25° C.
  4. filtrationwas filtered
  5. customThe collected solid was re-crystallized from benzene/methanol