반응 #3209

반응 방정식

2-amino-6-methoxybenzoic acid

bis(trichloromethyl)carbonate

→

title compound

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

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   기타whereupon a tan precipitate formed
2. 2
   온도cooled
3. 3
   여과filtered
4. 4
   온도cool
5. 5
   기타dried

실험 절차

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).

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