Acetic Anhydride → HCID 178473836, Verbindung

HRID 1486594Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1486594
F[C:2](F)(F)[C:3]([OH:5])=O.[Cl:8][C:9]1[CH:10]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:12]=[C:13]([Cl:15])[CH:14]=1.C(=O)(O)[O-].[Na+].C(OC(=O)C)(=O)C>C(#N)C>[Cl:15][C:13]1[CH:12]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][N:26]([C:3](=[O:5])[CH3:2])[CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:10]=[C:9]([Cl:8])[CH:14]=1

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178478184HCID 178478184, Verbindung

Produkt 1

HCID 178473836HCID 178473836, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a stirred suspension of N3-(3,5-dichlorophenyl)-N5-(piperidin-4-yl)-1H-1,2,4-triazole-3,5-diamine 2,2,2-trifluoroacetate (50 mg, 0.113 mmol) in acetonitrile (5 mL), was added saturated sodium bicarbonate solution (5 mL) and acetic anhydride (14 mg, 0.136 mmol). The reaction mixture was stirred overnight at rt. The solution was extracted with EtOAc (3×10 mL) and dried with sodium sulfate. Removal of solvent gave the crude product, which was purified by flash chromatography to give 35 mg (84%) desired product as a white solid. MS +m/z: 369.0 (M+H)+

Aufarbeitung

  1. extractionThe solution was extracted with EtOAc (3×10 mL)
  2. dry with materialdried with sodium sulfate
  3. customRemoval of solvent
  4. customgave the crude product, which
  5. customwas purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3a2caf15307d4b4381b6663471d222b8
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09428469B2

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