Reaktion #325658

Reaktionsgleichung

2-Amino-4-nitro-phenol

THF

2-Bromo-2-methyl-propionyl bromide

→

2-Bromo-N-(2-hydroxy-5-nitro-phenyl)-2-methyl-propionamide

Lösungsmittel

Et3N

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONthen poured into ice
2. 2
   ExtraktionThe aqueous phase was extracted by EtOAc (50 mL×4)
3. 3
   SonstigeThe organic layer was dried
4. 4
   Einengenconcentrated
5. 5
   SonstigeThe desired product was crystallized from EtOAc

Vorschrift

2-Amino-4-nitro-phenol (3.08 g, Aldrich) was stirred with THF (30 ml, Aldrich) in an ice bath. 2-Bromo-2-methyl-propionyl bromide (2.47 ml, Aldrich) and Et3N (2.0 g, Aldrich) was slowly added via syringe. The mixture was stirred for 45 min then poured into ice. The aqueous phase was extracted by EtOAc (50 mL×4). The organic layer was dried and concentrated. The desired product was crystallized from EtOAc. (Chem. Pharm. Bull 1996, 44(1) 103-114).

Quelle