تفاعل #2335930

ord-18b3b16242f14763a911f42e841dd28e

معادلة التفاعل

O
water
COCC(=O)Cl
methoxyacetyl chloride
CCNc1cccc(N)c1C#N
2-amino-6-(ethylamino)benzonitrile
c1ccncc1
pyridine
CCNc1cccc(NC(=O)COC)c1C#N
title compound
CCNc1cccc(NC(=O)COC)c1C#N
2-(ethylamino)-6-(methoxyacetylamino)benzonitrile

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةis cooled in an ice bath
  2. 2
    استخلاصthe mixture is extracted with methylene chloride
  3. 3
    تجفيفThe organic layer is dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  5. 5
    أخرىThe resulting crude crystals are recrystallized from ethyl acetate-hexane

الإجراء التجريبي

To a solution of 2-amino-6-(ethylamino)benzonitrile (3.4 g) in methylene chloride (50 ml) is added pyridine (2.4 ml), and thereto is added dropwise methoxyacetyl chloride (2.8 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethyl acetate-hexane to give the title compound (3.2 g) having the following physical properties.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05041462uspto-grants-1991_08