تفاعل #84878

ord-05d02b578f3241d1adb7583028d7eb0a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصwas extracted twice with ethyl acetate
  2. 2
    تجفيفThe combined organic phases were dried over sodium sulphate
  3. 3
    ترشيحfiltered
  4. 4
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

At 0° C., 5.2 ml (29.8 mmol, 3 eq.) of N,N-diisopropylethylamine and 0.62 g (purity 80%, 9.92 mmol, 1.0 eq.) of hydrazine monohydrate were added to a solution of 2.0 g (9.92 mmol) of 4-nitrobenzenecarboximidamide monohydrochloride in 20 ml of methanol, and the mixture was stirred at RT for 64 h. The reaction mixture was then added to 10% strength sodium chloride solution and, after addition of ethyl acetate and phase separation, was extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 1.7 g (93% of theory)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434690B2uspto-grants-2016_09