Ammonia → HCID 51347693, Verbindung

HRID 591228Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 591228
Cl[C:2]1[N:7]2[N:8]=[C:9]([S:11][CH3:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:13])[CH:3]=1.[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([S:21]([F:26])([F:25])([F:24])([F:23])[F:22])=[CH:17][CH:16]=1.N>C(O)C>[CH3:13][C:4]1[CH:3]=[C:2]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([S:21]([F:26])([F:22])([F:23])([F:24])[F:25])=[CH:17][CH:16]=2)[N:7]2[N:8]=[C:9]([S:11][CH3:12])[N:10]=[C:6]2[N:5]=1

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 27791904-Aminophenylsulphur pentafluorideHCID 10512843HCID 10512843, Verbindung2×

Produkt 1

HCID 51347693HCID 51347693, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a suspension of 7-chloro-5-methyl-2-(methylthio)[1,2,4]triazolo[1,5-a]pyrimidine (Intermediate 8, (0.2 g, 0.932 mmol)), in ethanol (10 mL), 4-aminophenylsulfur pentafluoride (MANCHESTER, 0.204 g, 0.932 mmol) was added and the mixture was stirred at room temperature until reaching completion. Anhydrous ammonia (0.133 mL, 0.932 mmol) was then added to the mixture and solvent was removed in vacuo. The crude mixture was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures form 95:5 to 40:60%). Upon collection of the appropriate fractions, the title compound was obtained as a light yellow solid.

Aufarbeitung

  1. customwas removed in vacuo
  2. customThe crude mixture was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures form 95:5 to 40:60%)
  3. customUpon collection of the appropriate fractions

Quellen und Nachweise

ORD-Eintrag
ord-e985b8936280459ca7ebdbc34a3e9fac
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09238653B2

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