Hydrochloric Acid → HCID 59649710, Verbindung

HRID 2081079

Reaktionsgleichung

Reaktionsgleichung von HRID 2081079
COC[O:4][C:5]1[CH:6]=[C:7]([C:12]2[N:13]=[N:14][N:15]([CH3:17])[CH:16]=2)[CH:8]=[CH:9][C:10]=1[CH3:11].Cl>O1CCCC1CCCO.O1CCOCC1>[CH3:11][C:10]1[CH:9]=[CH:8][C:7]([C:12]2[N:13]=[N:14][N:15]([CH3:17])[CH:16]=2)=[CH:6][C:5]=1[OH:4]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 59649725HCID 59649725, Verbindung

Produkt 1

HCID 59649710HCID 59649710, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 130202-Furanpropanol, tetrahydro-LösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 4-(3-methoxymethoxy-4-methyl-phenyl)-1-methyl-1H-[1,2,3]triazol (0.57 g, 2.44 mmol) (from Example 20 supra) in tetrahydrofuran-2-propanol (1:1, 20 mL) was added HCl in dioxane (4 M, 8 mL) (Aldrich). The reaction mixture was stirred at room temperature for 2 days. The solution was concentrated. The residue was diluted with ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and brine, dried (MgSO4) and concentrated. The residue was recrystallized from ethyl acetate-hexanes and dried to give 2-methyl-5-(1-methyl-1H-[1,2,3]triazol-4-yl)-phenol. (Yield 0.24 g, 52%).

Aufarbeitung

  1. concentrationThe solution was concentrated
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with saturated aqueous sodium bicarbonate solution and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customThe residue was recrystallized from ethyl acetate-hexanes
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2fe3fde0ac6d4c5c9ba4aa5954be6d82
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07932390B2

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