Methanol → HCID 66815646, Verbindung

HRID 2367923Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2367923
[C:1]([O:5][C:6](=[O:27])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[N:21]=[C:20]([C:23]([O:25]C)=[O:24])[CH:19]=[CH:18]2)([CH3:4])([CH3:3])[CH3:2].CO>C(OCC)(=O)C.CCCCCC.C(O)(=O)C>[C:1]([O:5][C:6](=[O:27])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[N:21]=[C:20]([C:23]([OH:25])=[O:24])[CH:19]=[CH:18]2)([CH3:4])([CH3:2])[CH3:3]

Komponenten

4

Edukt 2

HCID 887MethanolHCID 67773395HCID 67773395, Verbindung

Produkt 1

HCID 66815646HCID 66815646, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21901998Ethyl acetate hexane acetic acidLösungsmittel

Versuchsvorschrift

To a solution of compound 1 (540 mg, 1.45 mmol, 1 eq.) in MeOH (3 mL) NaOH (116 mg, 2.9 mmol, 2 eq.) was added as, a concentrated aqueous solution, and the mixture was stirred at room temperature. The reaction was monitored by TLC (ethyl acetate/hexane/acetic acid, 1:1:0.01). Upon completion the volatiles were removed in vacuo and ethyl acetate added. The solution was washed with NaH2PO4 buffer (pH 5, 1M) and brine, dried over Na2SO4, and concentrated in vacuo to give 446 mg of crude 2, which was used directly in the next step. MS m/z 360 [M−H]+

Aufarbeitung

  1. customUpon completion the volatiles were removed in vacuo and ethyl acetate
  2. additionadded
  3. washThe solution was washed with NaH2PO4 buffer (pH 5, 1M) and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customto give 446 mg of crude 2, which

Quellen und Nachweise

ORD-Eintrag
ord-8a3ab6d0e0ef45a09927719a63c9fab4
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08703700B2

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