反応 #3209

反応方程式

2-amino-6-methoxybenzoic acid

bis(trichloromethyl)carbonate

→

title compound

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

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他whereupon a tan precipitate formed
2. 2
   温度cooled
3. 3
   ろ過filtered
4. 4
   温度cool
5. 5
   その他dried

実験手順

To a stirred warm (50° C.) solution of 2-amino-6-methoxybenzoic acid (2.70 g, 16.2 mM) in tetrahydrofuran (25 mL) under a nitrogen atmosphere was added bis(trichloromethyl)carbonate (1.60 g, 5.38 mM), whereupon a tan precipitate formed. The reaction mixture was maintained at 50° C. for 30 min, cooled, rewarmed to 50° C. for 30 min, filtered cool and dried to provide the title compound (2.95 g, 94.6%) as an off-white solid; MS(CI): 194 (M+H).

出典