Ammonia → HCID 58497086, Verbindung

HRID 2283937Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2283937
[Cl:1][C:2]1[C:7]([CH2:8][CH3:9])=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[NH3:11]>C(O)CCC>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([NH2:11])[C:7]=1[CH2:8][CH3:9]

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 218284324,6-Dichloro-5-ethylpyrimidine

Produkt 1

HCID 58497086HCID 58497086, VerbindungAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a mixture of 4,6-Dichloro-5-ethylpyrimidine (22.5 g, 0.12 mol) in 1-butanol (70 mL) in a 1L glass pressure tube was added aqueous ammonia (26%, 150 mL) at RT. The vessel was sealed and heated to 100° C. for 12 h. The reaction mixture was cooled to RT, the resulted solid was filtered, washed with water (50 mL) and dried under vacuum to afford the titled compound (11.0 g, 55%) as white solid. LCMS: Mass found (M+, 158.0). 1H NMR (400 MHz, CDCl3) 8.02 (s, 1H), 7.10 (bs, 2H), 2.57-2.50 (m, 2H), 1.03-0.99 (m, 3H).

Aufarbeitung

  1. customThe vessel was sealed
  2. temperatureThe reaction mixture was cooled to RT
  3. filtrationthe resulted solid was filtered
  4. washwashed with water (50 mL)
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-aaad08d38d1f4cea9c598189671b3451
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09145392B2

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