Urea → HCID 12023321, Verbindung

HRID 2236567Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2236567
[C:1]([CH2:4][C:5]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:6]=1[C:7](O)=[O:8])(O)=[O:2].[NH2:15]C(N)=O>>[Cl:14][C:12]1[CH:13]=[C:5]2[C:6](=[CH:10][CH:11]=1)[C:7](=[O:8])[NH:15][C:1](=[O:2])[CH2:4]2

Komponenten

3

Edukt 2

HCID 1176UreaHCID 3340352-(Carboxymethyl)-4-chlorobenzoic acid

Produkt 1

HCID 12023321HCID 12023321, VerbindungAusbeute 34 %

Versuchsvorschrift

An amount of 2-(carboxymethyl)-4-chlorobenzoic acid (8.4 g, 39.14 mmol) and 2.82 g (47 mmol) of urea is vigorously stirred at 160° C. Solids were melted, boiled and hardened after 15 min. Continue to heat and blow nitrogen through to remove water generated from reaction until total dryness. After cooling, the solid is ground to fine powder. After successively washing with saturated NaHCO3 solution, water, methanol, ether and hexane, the powder is dried in oven (60° C.) overnight to give 2.6 g (34.0% yield) of light yellow solid: MS (ESI) m/z 194.0 (M−H)−1 Analysis for C9H6ClNO2, Calcd: C, 55.26; H, 3.09; N, 7.16. Found: C, 54.86; H, 2.96; N, 7.12

Aufarbeitung

  1. temperatureto heat
  2. customto remove water
  3. customgenerated from reaction until total dryness
  4. temperatureAfter cooling
  5. washAfter successively washing with saturated NaHCO3 solution, water, methanol, ether and hexane
  6. customthe powder is dried in oven (60° C.) overnight
  7. customto give 2.6 g (34.0% yield) of light yellow solid

Quellen und Nachweise

ORD-Eintrag
ord-4a9437c76226460d995d0aaa045cb8c5
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07713994B2

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