O-Xylene → HCID 178507852, Verbindung

HRID 26407

Reaktionsgleichung

Reaktionsgleichung von HRID 26407
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4](Cl)[N:3]=1.CC1C=CC=CC=1C.[NH:19]1[CH2:24][CH2:23][CH:22]=[CH:21][CH2:20]1.[OH-].[Na+]>O>[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:19]2[CH2:20][CH:21]=[CH:22][CH2:23][CH2:24]2)[N:3]=1

Komponenten

6

Edukt 4

HCID 7237O-XyleneHCID 127501,2,3,6-TetrahydropyridineHCID 14798Sodium HydroxideHCID 178507684HCID 178507684, Verbindung

Produkt 1

HCID 178507852HCID 178507852, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

155 G. of 2,4-diamino-6-chloropyrimidine-3-oxide are mixed under an argon atmosphere with 640 ml. of o-xylene and 260 ml. of 1,2,5,6-tetrahydropyridine and the mixture is stirred. The mixture is then heated to reflux for 30 minutes, the internal temperature rising from 115° C. to 123° C. The mixture is then cooled to 5° C., treated with 40 g. of sodium hydroxide in 400 ml. of water and stirred at 5° C. for 1 hour. The precipitate formed is filtered off, washed with 200 ml. of water and recrystallized from 3000 ml. of water, there being obtained pure 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide, having a melting point of 263°-265° C. (decomposition).

Aufarbeitung

  1. temperatureThe mixture is then heated
  2. temperatureto reflux for 30 minutes
  3. customrising from 115° C. to 123° C
  4. additiontreated with 40 g
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with 200 ml
  8. customof water and recrystallized from 3000 ml

Quellen und Nachweise

ORD-Eintrag
ord-565ac54cd7544d309a3fc4960985e1dc
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150131

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