反応 #5616

反応方程式

phosphorus pentachloride

4,5-diacetoxy-2-pyridinecarboxylic acid

diisopropyl ether

→

4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride

収率 158.5%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.WAITThe stirring was continued for an hour at -18°~12° C
2. 2
   その他The resulting precipitates
3. 3
   ろ過were collected by filtration
4. 4
   洗浄washed with diisopropyl ether
5. 5
   乾燥dried over phosphorus pentoxide

実験手順

To a suspension of phosphorus pentachloride (4.6 g) in methylene chloride (40 ml) was added 4,5-diacetoxy-2-pyridinecarboxylic acid (4.5 g) at -20° C. with stirring. The stirring was continued for an hour at -18°~12° C. To the reaction mixture was added diisopropyl ether (80 ml) below 0° C. The resulting precipitates were collected by filtration, washed with diisopropyl ether and dried over phosphorus pentoxide to give 4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride (5.15 g).

出典