2-(Methylamino)ethanol → 6-((2-hydroxyethyl)(methyl)amino)pyrimidine-2,4(1H,3H)-dione

HRID 873037Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 873037
[CH3:1][NH:2][CH2:3][CH2:4][OH:5].Cl[C:7]1[NH:12][C:11](=[O:13])[NH:10][C:9](=[O:14])[CH:8]=1>[I-].[K+].O>[OH:5][CH2:4][CH2:3][N:2]([CH3:1])[C:7]1[NH:12][C:11](=[O:13])[NH:10][C:9](=[O:14])[CH:8]=1

Komponenten

5

Edukt 2

HCID 80162-(Methylamino)ethanolHCID 732726-Chlorouracil

Produkt 1

HCID 867241596-((2-hydroxyethyl)(methyl)amino)pyrimidine-2,4(1H,3H)-dioneAusbeute 75,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 4875Potassium IodideKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a microwave reaction tube 2-(methylamino)ethanol (1.652 g, 22 mmol), 6-chloropyrimidine-2,4(1H,3H)-dione (1.465 g, 10 mmol), potassium iodide (KI) (0.017 g, 0.1 mmol) and water (20 mL) were added. The mixture was heated to 120° C. by microwave (Biotage Initiator) and stirred for 2 h. Then the solution was concentrated in vacuo to remove all the water. EtOH (10 mL) was added to the resultant residue. The suspension was filtered and the filter cake was collected to afford the title compound as a light-yellow solid (1.390 g, 75% yield),

Aufarbeitung

  1. additionwere added
  2. concentrationThen the solution was concentrated in vacuo
  3. customto remove all the water
  4. additionEtOH (10 mL) was added to the resultant residue
  5. filtrationThe suspension was filtered
  6. customthe filter cake was collected

Quellen und Nachweise

ORD-Eintrag
ord-db23b6ba5cb1450290b0431a9021b412
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975400B2

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