反应详情

2-Amino-5-iodobenzoic acid (25.4 g, 96.6 mmol) was added in portions to cold acetic anhydride (100 mL). The suspension was first stirred without cooling, then the resulting thick precipitate was heated at reflux for 1 h (red solution). The product crystallized spontaneously upon cooling. After stirring in ice for 30 min, the crystals were filtered off and washed twice with heptane. The crystals were thoroughly dried at 0.1 mbar/50° C. One obtained 25.1 g (90%) of beige crystals. MS: m/z=287 (M).

1. temperaturewithout cooling
2. temperaturethe resulting thick precipitate was heated
3. temperatureat reflux for 1 h (red solution)
4. customThe product crystallized spontaneously
5. temperatureupon cooling
6. stirringAfter stirring in ice for 30 min
7. filtrationthe crystals were filtered off
8. washwashed twice with heptane
9. customThe crystals were thoroughly dried at 0.1 mbar/50° C