Reaktion #9272

ord-7e0ae6c8d873495eb76902d9b21f0789

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure
  2. 2
    Sonstigethe crude reaction mixture
  3. 3
    Sonstigewas purified by preparative HPLC
  4. 4
    SonstigeLC/MS 2.86 min, 341 (M+1)

Vorschrift

About 0.2 g of 2-[(ethylamino)Carbonyl]amino-1,3-benzothiazole-6-carboxylic acid was dissolved into about 20 mL dichloromethane and about 0.2 mL triethylamine. Added about 1 eq of the appropriate amine followed by about 0.3 g of 1-ethyl-3-(3-dimethylaminopropyl)Carbodiimide hydrochloride then stirred at room temperature for about 12–24 hours. The solvent was removed under reduced pressure then the crude reaction mixture was purified by preparative HPLC. 1H NMR 1.10 (t, 3H), 3.2 (m, 2H), 6.76 (br s, 11), 7.10 (m, 1H), 7.36 (m, 2H), 7.70 (d, 1H), 7.79 (d, 2H), 7.97 (m, 1H), 8.5 (s, 1H), 10.23 (s, 1H), 10.9 (br s, 1H); LC/MS 2.86 min, 341 (M+1);

Quelle

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