反応 #3197

反応方程式

2-amino-6-chlorobenzoic acid

bis(trichloromethyl)carbonate

→

title compound

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

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   ろ過the precipitate was collected by filtration
2. 2
   洗浄washed with ether
3. 3
   その他Air drying

実験手順

To a stirred warm (50° C.) solution of 2-amino-6-chlorobenzoic acid (2.00 g, 11.7 mM) in tetrahydrofuran (20 mL) was added bis(trichloromethyl)carbonate (1.20 g, 4.10 mM). A vigorous gas evolution ensued along with the formation of a precipitate. The reaction mixture was allowed to cool to room temperature and the precipitate was collected by filtration and washed with ether. Air drying gave the title compound as a tan solid (2.0 g, 87%); MS(CI): 198 (M+H).

出典