Methanol → HCID 68533538, Verbindung

HRID 736703Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 736703
[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13]C)=[O:12])=[C:9]([F:17])[CH:8]=1.[OH-].[Li+].CO>O1CCCC1.O>[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:16]=[CH:15][C:10]([C:11]([OH:13])=[O:12])=[C:9]([F:17])[CH:8]=1

Komponenten

6

Edukt 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68533674HCID 68533674, Verbindung

Produkt 1

HCID 68533538HCID 68533538, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of EXAMPLE 22A (1.9 g) in tetrahydrofuran (10 mL) and water (5 mL) was added lithium hydroxide (1 g) in water (5 mL). Methanol was added until homogeneous and the solution stirred at ambient temperature for 4 hours. The mixture was concentrated to 5 mL and the residue acidified to pH 2 with 2 N hydrochloric acid. Ethyl acetate and water were added and the organic phase separated, washed with water, dried over magnesium sulfate, filtered and concentrated to give the title compound (1.7 g, 95%). MS (DCI): m/z 227 (M+H)+.

Aufarbeitung

  1. concentrationThe mixture was concentrated to 5 mL
  2. additionEthyl acetate and water were added
  3. customthe organic phase separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-e3d590cd19394831acb99e28ea1048b2
Quelldatensatz
uspto-grants-2009_09
Patentnummer
US07595406B2

Notizen zur Reaktion

Wird geladen…