반응 #159090

반응 방정식

4,4′-Dibromo-2′-methoxy-biphenyl-2-ylamine

NaNO2

Urea

→

3,7-dibromo-dibenzofuran

수율 71.1%

용매

water

H2SO4

water

water

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred for 12 hours
2. 2
   온도was heated at 70° C. for 24 hours
3. 3
   온도The mixture was cooled to 25° C.
4. 4
   여과was filtered
5. 5
   기타The collected solid was re-crystallized from benzene/methanol

실험 절차

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).

출처