반응 #44423

ord-a5c35d0dd7fe4a1aa842846ec4e1bb61

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 5 h
  2. 2
    여과the mixture is filtered
  3. 3
    농축the filtrate is concentrated in vacuo
  4. 4
    workup.ADDITIONEthanol is added to the residue
  5. 5
    workup.STIRRINGthe mixture is stirred
  6. 6
    여과The solid is filtered off with suction
  7. 7
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737144B2uspto-grants-2010_06