Reaktion #9194
ord-68f4737b6c484d558c81c99a24e5ed31
Reaktionsgleichung
6-chloro-1,3-benzothiazol-2-amine
EtNCO
triethylamine
→
N-(6-Chloro-1,3-benzothiazol-2-yl)-N′-ethylurea
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigeto react at about 80° C. for about 8 hours
- 2SonstigeThe reaction solvent was then removed in vacuo
- 3SonstigeThe solids were isolated by filtration
- 4Waschenwashed with ether
- 5SonstigeThe product was then dried in vacuo
Vorschrift
Three grams of 6-chloro-1,3-benzothiazol-2-amine was dissolved in about 50 mL DMF. Next, about 2.5 mL of EtNCO was added followed by about 3.2 mL of triethylamine. The solution was allowed to react at about 80° C. for about 8 hours. The reaction solvent was then removed in vacuo and the crude oil was taken up in ether. The solids were isolated by filtration and washed with ether. The product was then dried in vacuo. 1H NMR 1.09 (t, 3H, J=7.2 Hz), 3.19 (m, 2H), 6.74 (br s, 1H), 7.37 (d, 1H, J=8.58 Hz), 7.60 (d, 1H, J=8.59 Hz), 8.01 (s, 1H), 10.8 (br s, 1H). LCMS: R.T. 2.3 min, MH-254 m/z.