Methanol → HCID 15521806, Verbindung

HRID 356809

Reaktionsgleichung

Reaktionsgleichung von HRID 356809
O[CH:2]([OH:6])[C:3](=[O:5])[CH3:4].N1[CH:12]=[CH:11][CH:10]=CC=1.[C:13]([O:18]C(=O)C(C)C)(=[O:17])[CH:14]([CH3:16])[CH3:15].[CH3:24][OH:25]>CN(C)C1C=CN=CC=1.C(OCC)(=O)C>[C:13]([O:18][CH2:4][C:3]([CH2:2][O:6][C:24](=[O:25])[CH:11]([CH3:10])[CH3:12])=[O:5])(=[O:17])[CH:14]([CH3:16])[CH3:15]

Komponenten

7

Edukt 4

HCID 887MethanolHCID 1049PyridineHCID 7346Isobutyric anhydrideHCID 131809821,1-Dihydroxypropan-2-one

Produkt 1

HCID 15521806HCID 15521806, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A 100 ml reaction vessel was charged with 4.18 g of dihydroxyacetone (monomer), 11.2 ml of pyridine and 10 mg of 4-dimethylaminopyridine and the mixture was stirred at room temperature. Thereto was added dropwise 16.7 ml of isobutyric anhydride over 30 minutes. After the dropping, the resulting liquid was further stirred for 1 hour and then 1 ml of methanol was added thereto and the resulting liquid was further stirred for 1 hour. To the reaction mixture was added ethyl acetate and the organic layer was separated. The organic layer was washed with water and further washed with saturated aqueous solution with sodium bicarbonate and 1N HCl. Then, the solvent was removed under reduced pressure. The residue was distilled under reduced pressure to give 7.47 g of the desired compound.

Aufarbeitung

  1. customA 100 ml reaction vessel
  2. stirringAfter the dropping, the resulting liquid was further stirred for 1 hour
  3. stirringthe resulting liquid was further stirred for 1 hour
  4. customthe organic layer was separated
  5. washThe organic layer was washed with water
  6. washfurther washed with saturated aqueous solution with sodium bicarbonate and 1N HCl
  7. customThen, the solvent was removed under reduced pressure
  8. distillationThe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a997e571454d4d2ca8243fa3c1bb3cc0
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840553

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