反応 #6918

反応方程式

2-amino-4-fluoro-5-iodo-benzoic acid

trichloromethylchloroformate

→

title compound

収率 90.4%

4-Fluoro-5-iodo-isatoic anhydride

収率 90.4%

溶媒

—

hexanes

dioxane

反応条件

後処理

1. 1
   その他equipped with a magnetic stir bar
2. 2
   温度reflux condenser
3. 3
   温度heated
4. 4
   温度to reflux for 16 hours
5. 5
   温度to cool
6. 6
   ろ過The solid was collected by suction filtration
7. 7
   洗浄washed with an additional 0.5 litres of hexanes
8. 8
   その他dried under vacuum at room temperature

実験手順

Anhydrous dioxane (0.5 litres), 2-amino-4-fluoro-5-iodo-benzoic acid (46 grams, 164 mmoles), and trichloromethylchloroformate (97.4 grams, 492 mmoles) were added to a one litre one neck flask equipped with a magnetic stir bar and reflux condenser. The solution was placed under anhydrous nitrogen, stirred and heated to reflux for 16 hours. The reaction mixture was allowed to cool and was poured into one litre of hexanes. The solid was collected by suction filtration, washed with an additional 0.5 litres of hexanes, and dried under vacuum at room temperature to yield 45.5 grams (90%) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ: 11.86(s, 1H), 8.24(d, 1H), 6.84(d, 1H). ESI-MS m/z 308 (M+1).

出典