Reaktion #9267

ord-0c31608d9ad04d16b80f61e52ee18c38

Reaktionsgleichung

Nc1nc2ccc(Br)cc2s1
6-bromo-1,3-benzothiazol-2-amine
CCN=C=O
ethylisocyanate
CCN(CC)CC
triethylamine
CCNC(=O)Nc1nc2ccc(Br)cc2s1
N-(6-Bromo-1,3-benzothiazol-2-yl)-N′-ethylurea

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthen cooled to RT
  2. 2
    SonstigeThe solvent is removed in vacuo
  3. 3
    Waschenthe solids are washed well with ether
  4. 4
    SonstigeThe product is further purified by column chromatography

Vorschrift

About 0.75 g of 6-bromo-1,3-benzothiazol-2-amine (crude) is dissolved in about 15 mL DMF. About 0.5 mL of ethylisocyanate is added followed by about 0.9 mL triethylamine and the solution is heated to about 80° C. under good agitation. The solution is allowed to stir for about 4 hours then cooled to RT. The solvent is removed in vacuo and the solids are washed well with ether. The product is further purified by column chromatography.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091227B2uspto-grants-2006_08