反应详情

To a cooled (0° C.) brown solution of 4,6-dimethoxy anthranilic acid (76.0 g, 0.385 mol), prepared as in Example 2, in tetrahydrofuran (1.3 L) was added triphosgene (40.0 g, 0.135 mol) in portions over a 20 min period. After 30 min, the reaction was warmed to room temperature and stirred for an additional 1.5 h. The reaction mixture was poured into an Erlenmeyer flask containing water and cooled to 0° C. with an ice bath. Additional water was added to facilitate the stirring of the thick solid formed. After stirring for 30 min, the reaction mixture was filtered to give a beige solid. The solid was washed with water, air-dried, and then dried under high vacuum to give 79.2 g (92%) of the isatoic anhydride.

1. temperatureTo a cooled
2. additionThe reaction mixture was poured into an Erlenmeyer flask
3. temperaturecooled to 0° C. with an ice bath
4. stirringstirring of the thick solid
5. customformed
6. stirringAfter stirring for 30 min
7. filtrationthe reaction mixture was filtered
8. customto give a beige solid
9. washThe solid was washed with water
10. customair-dried
11. customdried under high vacuum