Reaktion #3226

Reaktionsgleichung

water

2-amino-4-chloro-6-trifluoromethylbenzoic acid

bis(trichloromethyl)carbonate

→

title compound

5-Chloro-7-trifluoromethyl-2H-3,1-benzoxazine-2,4(1H)-dione

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe resulting mixture extracted with ethyl acetate
2. 2
   TrocknenThe combined extracts were dried (MgSO4)
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated

Vorschrift

To a stirred solution of 2-amino-4-chloro-6-trifluoromethylbenzoic acid (0.53 g, 2.2 mM) in dry tetrahydrofuran (6 mL) under a nitrogen atmosphere was added bis(trichloromethyl)carbonate (0.218 g, 0.734 mM). The resulting solution was stirred at room temperature for 2 hr, poured into water and the resulting mixture extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered and concentrated to leave the title compound as a tan solid; MS(CI): 266 (M+H).

Quelle