تفاعل #40560

ord-9feb74f319eb4940b9784589c395aa8d

معادلة التفاعل

O=C(O)c1cc(Cl)n[nH]c1=O
6-chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid
Nc1ccccc1N
ortho-phenylenediamine
CCN=C=NCCCN(C)C.Cl
1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride
Nc1ccccc1NC(=O)c1cc(Cl)n[nH]c1=O
6-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid (2-amino-phenyl)amide

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONare added
  2. 2
    workup.DISTILLATIONFor workup, the solvent is distilled off
  3. 3
    أخرىis suspended in water at 70° C
  4. 4
    ترشيحThe precipitate is filtered off
  5. 5
    غسيلwashed several times with water
  6. 6
    أخرىdried in vacuo

الإجراء التجريبي

30.5 g of 6-chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid, 18 g of ortho-phenylenediamine and 2 g of DMAP are dissolved in 800 ml of DMF, at room temperature 32.2 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride are added, and the resulting solution is stirred at room temperature for 4 hours. For workup, the solvent is distilled off and the residue is suspended in water at 70° C. The precipitate is filtered off, washed several times with water and then dried in vacuo.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07727989B2uspto-grants-2010_06