تفاعل #3209

معادلة التفاعل

2-amino-6-methoxybenzoic acid

bis(trichloromethyl)carbonate

→

title compound

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

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىwhereupon a tan precipitate formed
2. 2
   درجة الحرارةcooled
3. 3
   ترشيحfiltered
4. 4
   درجة الحرارةcool
5. 5
   أخرىdried

الإجراء التجريبي

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).

المصدر