反应详情

A mixture of 2-amino-5-iodobenzoic acid (25 g, 95.05 mmol) and triphosgene (77.1 g, 260.4 mmol) in dioxane (316 mL) was heated to reflux for 8 h. The resulting solid was filtered and washed with diethyl ether to give 28.1 g of the title compound, 1H NMR (300 MHz, Me2SO-d6): δ6.96 (d,1H); 8.02 (dd,1H); 8.13 (d,1H); 11.82 (br s,1H); m/e 288 deprotonated parent molecular ion (m/e) measured by mass spectrometry using atmospheric pressure chemical ionization in the negative ion mode (APCI-).

1. temperaturewas heated
2. temperatureto reflux for 8 h
3. filtrationThe resulting solid was filtered
4. washwashed with diethyl ether