Reaktion #587368

Reaktionsgleichung

N,N-Dimethylcarbamoyl chloride

1-(4-bromo-2-fluorophenyl)methanamine

triethylamine

→

N′-(4-bromo-2-fluorobenzyl)-N,N-dimethylurea

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe ice-water bath was removed
2. 2
   WaschenThe mixture was washed with water and brine
3. 3
   TrocknenThe organic layer was dried over Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue (253 mg, 91.9%) was directly used in next step without further purification

Vorschrift

N,N-Dimethylcarbamoyl chloride (101 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.10 mmol) in methylene chloride (5 mL) at 0° C., followed by 4-dimethylaminopyridine (0.012 g, 0.1 mmol). After 10 min, the ice-water bath was removed and the mixture was stirred overnight at RT. The mixture was washed with water and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (253 mg, 91.9%) was directly used in next step without further purification. LCMS: (M+H)=276.9/274.9.

Quelle