Hydrazine hydrate (1:1) → HCID 20805788, Verbindung

HRID 631862

Reaktionsgleichung

Reaktionsgleichung von HRID 631862
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.O.[NH2:16][NH2:17]>O1CCOCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:16][NH2:17])[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 2415542,4-Dichloro-6-phenylpyrimidine

Produkt 1

HCID 20805788HCID 20805788, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 2,4-dichloro-6-phenylpyrimidine (224 mg, 1 mmol) in 1 mL of 1,4-dioxane was added 300 uL of hydrazine hydrate. Stirring was continued at room temperature and the reaction monitored by thin layer chromatography (30% ethyl acetate/hexanes). When the starting material was consumed, 2 mL of water was added and the resultant precipitate was collected on a filter to afford 2-chloro-4-hydrazinyl-6-phenylpyrimidine as a yellow solid. The damp solid was suspended in 2 mL of ethanol, to which was added 220 mg of 4-trifluoromethoxybenzaldehyde. Within 5 minutes the solution became clear and then reprecipitated material. The product, 2-chloro-4-phenyl-6-(2-(4-(trifluoromethoxy)benzylidene)hydrazinyl)pyrimidine (XX), was collected by filtration and dried to afford 150 mg of a solid. ESI/MS 392.973, 395.002 (M+H).

Aufarbeitung

  1. customwas continued at room temperature
  2. customWhen the starting material was consumed
  3. addition2 mL of water was added
  4. customthe resultant precipitate was collected on
  5. filtrationa filter

Quellen und Nachweise

ORD-Eintrag
ord-d54cb5e4acd243dd83d68ec7933d6462
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09321735B2

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