反応 #82988

反応方程式

Acetic acid

acetic anhydride

cyclopropane-1,2,3-tricarboxylic acid

→

2,4-dioxo-3-oxabicyclo[3.1.0]hexane-6-carboxylic acid

収率 83.0%

反応条件

後処理

1. 1
   温度while heating
2. 2
   温度under reflux for 2 hours
3. 3
   濃縮concentrating the reaction solution into a half volume
4. 4
   ろ過filtering off
5. 5
   洗浄washing them with heptane
6. 6
   その他drying under reduced pressure

実験手順

Acetic acid (58.8 ml, 933 mmol) and acetic anhydride (20.4 ml, 185 mmol) were added to cyclopropane-1,2,3-tricarboxylic acid (24.4 g, 140 mmol), followed by reacting the mixture while heating under reflux for 2 hours, concentrating the reaction solution into a half volume, filtering off deposited crystals, washing them with heptane and drying under reduced pressure, to obtain 2,4-dioxo-3-oxabicyclo[3.1.0]hexane-6-carboxylic acid (18.1 g, 116 mmol, 83%).

出典