Sodium Hydroxide → N-(3-nitrophenyl)-4-(2-pyridyl)-2-pyrimidine-amine

HRID 440868

Reaktionsgleichung

Reaktionsgleichung von HRID 440868
CN(C)[CH:3]=[CH:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=O.[N+]([O-])(O)=O.[N+:18]([C:21]1[CH:22]=[C:23]([NH:27][C:28]([NH2:30])=[NH:29])[CH:24]=[CH:25][CH:26]=1)([O-:20])=[O:19].[OH-].[Na+]>C(O)(C)C>[N+:18]([C:21]1[CH:22]=[C:23]([NH:27][C:28]2[N:30]=[C:5]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=3)[CH:4]=[CH:3][N:29]=2)[CH:24]=[CH:25][CH:26]=1)([O-:20])=[O:19]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 5669933-Dimethylamino-1-(2-pyridyl)prop-2-en-1-oneHCID 1785125133-Nitrophenylguanidine Nitrate

Produkt 1

HCID 10708835N-(3-nitrophenyl)-4-(2-pyridyl)-2-pyrimidine-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

1 g (5.68 mmol)of 3-dimethylamino-1-(2-pyridyl)-2-propen-1-one [EP-A-233 461] is dissolved in 8 ml of isopropanol, and 1.38 g (5.68 mmol) of 3-nitrophenylguanidine nitrate are added. After the addition of 0.25 g (6.24 mmol) of sodium hydroxide, the yellow suspension is heated at reflux for 20 hours, then cooled to 0°, filtered and washed with 30 ml of isopropanol. The filtration residue is stirred in 15 ml of ethanol for 20 minutes, filtered and washed with a small amount of cold ethanol, yielding N-(3-nitrophenyl)-4-(2-pyridyl)-2-pyrimidine-amine; m.p. 213°-219°.

Aufarbeitung

  1. temperaturethe yellow suspension is heated
  2. temperatureat reflux for 20 hours
  3. temperaturecooled to 0°
  4. filtrationfiltered
  5. washwashed with 30 ml of isopropanol
  6. filtrationfiltered
  7. washwashed with a small amount of cold ethanol

Quellen und Nachweise

ORD-Eintrag
ord-b845d6dc1b164499ac1a9b2ef9232286
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05521184

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