反応 #657349

反応方程式

5-methoxyanthranilic acid

acetic anhydride

→

title compound

収率 77.0%

2-methyl-6-(methyloxy)-4H-3,1-benzoxazin-4-one

収率 77.0%

反応条件

後処理

1. 1
   温度before being cooled
2. 2
   濃縮concentrated under reduced pressure
3. 3
   濃縮The crude residue was then concentrated twice in the presence of toluene
4. 4
   ろ過before being filtered
5. 5
   洗浄washed with ether

実験手順

A solution of 5-methoxyanthranilic acid (7.8 g, 46.5 mmol) was refluxed in acetic anhydride (60 mL) for 2 h15 before being cooled and concentrated under reduced pressure. The crude residue was then concentrated twice in the presence of toluene before being filtered and washed with ether to yield to the title compound (6.8 g, 77% yield) as a beige solid; LC/MS: m/z 192 [M+H]+, Rt 1.69 min.

出典