O-Phenylenediamine → 6-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid (2-amino-phenyl)amide

HRID 12282노트

반응식

HRID 12282 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([OH:11])=O)[C:5](=[O:8])[NH:6][N:7]=1.[C:12]1([NH2:19])[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18].Cl.C(N=C=NCCCN(C)C)C>CN(C1C=CN=CC=1)C.CN(C=O)C>[NH2:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[NH:19][C:9]([C:4]1[C:5](=[O:8])[NH:6][N:7]=[C:2]([Cl:1])[CH:3]=1)=[O:11]

참가 물질

6

반응물 3

HCID 7243O-PhenylenediamineHCID 3340156-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 866116096-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid (2-amino-phenyl)amide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  1. additionare added
  2. distillationFor workup, the solvent is distilled off
  3. customis suspended in water at 70° C
  4. filtrationThe precipitate is filtered off
  5. washwashed several times with water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-9feb74f319eb4940b9784589c395aa8d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727989B2

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