تفاعل #54148

ord-134f974d07114d98b685b018028a437a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    أخرىa greenish-yellow precipitate separated
  3. 3
    درجة الحرارةat reflux for 30 minutes
  4. 4
    ترشيحThe greenish solid was filtered off
  5. 5
    غسيلwashed with cold methanol
  6. 6
    غسيلwashed
  7. 7
    أخرىvacuum dried

الإجراء التجريبي

To a slurry of 47.6 g (0.3 mol) of 2-chloro-5-nitropyridine in a mixture of 400 ml methanol and 60 ml water and cooled to 10° C. was added with cooling below 30° 86 g hydrazine (95 percent) over about 10 minutes. The solids first went into solution, then a greenish-yellow precipitate separated. The mixture was stirred at reflux for 30 minutes. The greenish solid was filtered off and washed with cold methanol. The solid was slurried in 200 ml of cold water, washed and vacuum dried. The yield was 40.1 g (87 percent).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04147544uspto-grants-1979_04