تفاعل #1168

ord-a6aacc5162fa4403a0432cd2a4af49bf

معادلة التفاعل

CC(=O)C(C#N)c1ccc(NC(=O)OC(C)(C)C)cc1
2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile
CCO
ethanol
CCOC(CNN)OCC
2,2-diethoxyethylhydrazine
Cl
hydrogen chloride
Cc1nn2cc[nH]c2c1-c1ccc(N)cc1.Cl
title compound
Cc1nn2cc[nH]c2c1-c1ccc(N)cc1.Cl
7-(4-Aminophenyl)-6-methyl-1H-imidazo[1,2-b]-pyrazole hydrochloride

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux for 2 hours
  3. 3
    درجة الحرارةthe whole mixture was heated
  4. 4
    درجة الحرارةunder reflux for a further 30 minutes
  5. 5
    درجة الحرارةAfter the mixture had been cooled
  6. 6
    أخرىto precipitate crystals
  7. 7
    ترشيحThese crystals were collected by filtration
  8. 8
    أخرىrecrystallized from ethanol

الإجراء التجريبي

A mixture of 2.5 g of 2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile, 20 ml of ethanol and 1.4 g of 2,2-diethoxyethylhydrazine was heated under reflux for 2 hours. 20 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, ethyl acetate was added to precipitate crystals. These crystals were collected by filtration and recrystallized from ethanol to give 1.4 g of the title compound as pale brown plates melting at 180°-190° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723481uspto-grants-1998_03