4-Chloroaniline → HCID 13121220, Verbindung

HRID 544385Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544385
Cl[C:2]1[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1>C(O)C>[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH:15][C:2]2[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=2)=[CH:13][CH:12]=1

Komponenten

4

Edukt 2

HCID 78124-ChloroanilineHCID 126003894-Chloro-5,6-dimethylpyrimidine

Produkt 1

HCID 13121220HCID 13121220, VerbindungAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

To 4.3 g (0.03 mole) of 4-chloro-5,6-dimethylpyrimidine were added 3.8 g (0.03 mole) of p-chloroaniline and about 10 ml of ethanol; the mixture wasthen heated at 130° C. for about 3 minutes. The reaction mixture quickly became a solution and then the hydrochloride of the desired compound precipitated as the solution was allowed to cool. The crystals thus obtained were separated and ground to a powder and then made alkalineby the addition of a dilute aqueous solution of sodium hydroxide. The insolubles were collected by filtration, washed with water and dried. The resulting crystals were recrystallised from benzene, to give 4.2 g (yield 60%) of the desired Compound No. 25, in the form of colourless needles melting at 170°-173° C.

Aufarbeitung

  1. customthe hydrochloride of the desired compound precipitated as the solution
  2. temperatureto cool
  3. customThe crystals thus obtained
  4. customwere separated
  5. additionground to a powder and then made alkalineby the addition of a dilute aqueous solution of sodium hydroxide
  6. filtrationThe insolubles were collected by filtration
  7. washwashed with water
  8. customdried
  9. customThe resulting crystals were recrystallised from benzene

Quellen und Nachweise

ORD-Eintrag
ord-3ae3fc4deb9d4c21b6c2263327f2acc2
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04450162

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