Reaktion #44423

ord-a5c35d0dd7fe4a1aa842846ec4e1bb61

Reaktionsgleichung

Cl
HCl
[Na]
sodium
CCOC(=O)CC(=O)OCC
Diethyl malonate
CCCNC(N)=O
n-propylurea
[Na]
sodium
CCCN1C(=O)CC(=O)NC1=O
1-Propylbarbituric acid

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 5 h
  2. 2
    Filtrationthe mixture is filtered
  3. 3
    Einengenthe filtrate is concentrated in vacuo
  4. 4
    workup.ADDITIONEthanol is added to the residue
  5. 5
    workup.STIRRINGthe mixture is stirred
  6. 6
    FiltrationThe solid is filtered off with suction
  7. 7
    Sonstigedried

Vorschrift

Metallic sodium (2.6 g, 113 mmol) is added to ethanol (60 ml). The mixture is stirred until the sodium has completely finished reacting. Diethyl malonate (116 ml, 105 mmol) and n-propylurea (10 g, 98 mmol) are then added and the mixture is stirred under reflux for 5 h. After conc. HCl (5 ml) and hot water (45 ml) have been added, the mixture is filtered and the filtrate is concentrated in vacuo. Ethanol is added to the residue and the mixture is stirred. The solid is filtered off with suction and dried.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737144B2uspto-grants-2010_06