Water → HCID 178489584, Verbindung

HRID 519508

Reaktionsgleichung

Reaktionsgleichung von HRID 519508
[CH3:1][C:2]1[NH:3][C:4]([NH2:7])=[N:5][N:6]=1.[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][C:11]1=O.C([BH3-])#N.[Na+].O>C(O)(=O)C>[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[NH:7][C:4]1[NH:3][C:2]([CH3:1])=[N:6][N:5]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1109982-MethoxycyclohexanoneHCID 5003444Sodium cyanoborohydrideHCID 178434112HCID 178434112, Verbindung

Produkt 1

HCID 178489584HCID 178489584, VerbindungAusbeute 52,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To a solution (50 mL) of 5-methyl-4H-1,2,4-triazol-3-amine (2.5 g) and 2-methoxycyclohexanone (3.9 g) in acetic acid was added sodium cyanoborohydride (8.1 g), and the mixture was stirred at room temperature for 16 hr. Water was added to the reaction mixture, and the solvent was evaporated under reduced pressure. The obtained residue was poured into saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with a mixed solvent of ethyl acetate and isopropyl alcohol (3:1). The obtained extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a colorless solid (2.8 g, 51%).

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe obtained residue was poured into saturated aqueous sodium hydrogen carbonate
  3. extractionthe mixture was extracted with a mixed solvent of ethyl acetate and isopropyl alcohol (3:1)
  4. extractionThe obtained extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a903266372b740278f2f8f42c22c86de
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09115136B2

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