تفاعل #66151

ord-5d8f74c42ce14871b154b69129200291

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was heated
  2. 2
    درجة الحرارةto reflux for 15 hours
  3. 3
    ترشيحfiltered
  4. 4
    تركيزThe filtrate was concentrated under reduced pressure

الإجراء التجريبي

To a solution of 1-(4,6-dimethyl-pyridin-2-yl)-4-(4-nitro-phenyl)-[1,4]diazepane (940 mg, 2.88 mmol) in ethyl acetate (25 mL) was added stannous chloride (3.90 g, 17.3 mmol) and ethanol (5 mL). The reaction mixture was heated to reflux for 15 hours then cooled to room temperature, basified with triethylamine and filtered. The filtrate was concentrated under reduced pressure to afford 4-[4-(4,6-dimethyl-pyridin-2-yl)-[1,4]diazepan-1-yl]-phenylamine (850 mg, 99%) as a brown solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524705B2uspto-grants-2013_09