Cyclopropylamine → N~2~,N~4~,N~6~-Tricyclopropyl-1,3,5-triazine-2,4,6-triamine

HRID 1448778Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1448778
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]2[CH2:11][CH2:10]2)[N:5]=[C:4]([NH:12][CH:13]2[CH2:15][CH2:14]2)[N:3]=1.[CH:16]1([NH2:19])[CH2:18][CH2:17]1>O1CCOCC1>[CH:16]1([NH:19][C:2]2[N:7]=[C:6]([NH:8][CH:9]3[CH2:11][CH2:10]3)[N:5]=[C:4]([NH:12][CH:13]3[CH2:15][CH2:14]3)[N:3]=2)[CH2:18][CH2:17]1

Komponenten

4

Edukt 2

HCID 69828CyclopropylamineHCID 6430808HCID 6430808, Verbindung

Produkt 1

HCID 57290175N~2~,N~4~,N~6~-Tricyclopropyl-1,3,5-triazine-2,4,6-triamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 20 g of 2-chloro-4,6-bis-cyclopropylamino-s-triazine, 10.1 g of cyclopropylamine and 80 ml of dioxan is heated at 140° C. in an autoclave for 22 hours. The reaction mixture is concentrated in vacuo to half its volume and 300 ml of water are added. The mixture is extracted with ethyl acetate, the product phase is dried over sodium sulfate and the solvents are removed in vacuo. The residue is recrystallised from dioxan/petroleum ether; melting point 75°-77° C.

Aufarbeitung

  1. concentrationThe reaction mixture is concentrated in vacuo to half its volume and 300 ml of water
  2. additionare added
  3. extractionThe mixture is extracted with ethyl acetate
  4. dry with materialthe product phase is dried over sodium sulfate
  5. customthe solvents are removed in vacuo
  6. customThe residue is recrystallised from dioxan/petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-be9ceb9e994d444193d71bfb373bd838
Quelldatensatz
uspto-grants-1980_02
Patentnummer
US04187305

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