Acetone → Deferiprone

HRID 273666

Reaktionsgleichung

Reaktionsgleichung von HRID 273666
[CH3:1][C:2]1O[CH:7]=[CH:6][C:4](=[O:5])[C:3]=1[OH:9].CC(C)=O.[CH3:14][NH2:15]>O>[CH3:14][N:15]1[CH:7]=[CH:6][C:4](=[O:5])[C:3]([OH:9])=[C:2]1[CH3:1]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 6329MethylamineHCID 8369Maltol

Produkt 1

HCID 2972DeferiproneAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Maltol (i.e. 2-methyl-3-hydroxypyran-4-one) 250 g) was dissolved in 25% aqueous methylamine (750 ml) and water (125 ml). The solution was pumped through the CMR (18 ml/min; 160°-2° C.; 900 kPa) and the hot reaction mixture passed directly into acetone (2.5 liters), cooled in an ice water bath. The crystalline product (146 g; 53% yield) was collected by filtration, and washed with acetone (2×250 ml). The corresponding literature method17 involved 6.5 hours at reflux, followed by laborious work up.

Aufarbeitung

  1. customwas pumped through the CMR (18 ml/min; 160°-2° C.; 900 kPa)
  2. temperaturecooled in an ice water bath
  3. filtrationThe crystalline product (146 g; 53% yield) was collected by filtration
  4. washwashed with acetone (2×250 ml)
  5. temperatureat reflux

Quellen und Nachweise

ORD-Eintrag
ord-69d841679ad645cdb75e4b78af585880
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387397

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