Sodium Hydroxide → Fibric acid

HRID 1429450

Reaktionsgleichung

Reaktionsgleichung von HRID 1429450
[CH3:1][C:2]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:8])[C:3]([O:5]CC)=[O:4].[OH-].[Na+]>CCO.O>[CH3:8][C:2]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:1])[C:3]([OH:5])=[O:4]

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 86476Deschloroclofibrate

Produkt 1

HCID 70343Fibric acidAusbeute 94,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of ethyl 2-methyl-2-phenoxypropanoate (2.0 g, 9.6 mmol) in EtOH (16 ml) was added a solution of NaOH (0.46 g, 11.5 mmol) in H2O (4 ml) at 26° C. The mixture was stirred for 30 min then concentrated. Water was added (20 mL) and washed with ethyl acetate (2×20 mL). The aqueous layer was acidified with 2N HCL until pH 3 and extracted with ethyl acetate (2×20 ml). The combined organic layers were washed with brine (30 mL), dried over Na2SO4 and concentrated to give the title compound (1.6 g, 94.1%) as a white solid which was used in next step without further purification.

Aufarbeitung

  1. concentrationthen concentrated
  2. additionWater was added (20 mL)
  3. washwashed with ethyl acetate (2×20 mL)
  4. extractionextracted with ethyl acetate (2×20 ml)
  5. washThe combined organic layers were washed with brine (30 mL)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-9b3a6e82d1de420196c0192095a3b22f
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08940726B2

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