تفاعل #159089

ord-b20646e410e74b57b9aedcd41fff593a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was refluxed for 7 hours
  2. 2
    ترشيحfiltered through a pad of CELITE
  3. 3
    غسيلThe CELITE pad was washed with ethanol
  4. 4
    تركيزThe combined solution was concentrated under reduced pressure

الإجراء التجريبي

To a suspension of 4,4′-dibromo-2-methoxy-2′-nitro-biphenyl (3.76 g, 9.8 mmol) and 5% Ru/C (400 mg) in ethanol (37 ml) at 65-70° C. was added dropwise a solution of hydrazine (4.6 ml, 59 mmol) in ethanol (5 ml). The mixture was refluxed for 7 hours and filtered through a pad of CELITE. The CELITE pad was washed with ethanol. The combined solution was concentrated under reduced pressure. Coevaporation with ethanol, EtOAc and DCM gave 4,4′-dibromo-2′-methoxy-biphenyl-2-ylamine as yellow solid (3.5 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822430B2uspto-grants-2014_09