反応 #69939

反応方程式

10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione

PCl5

→

5-chloro-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one

収率 139.7%

溶媒

chloroform

反応条件

後処理

1. 1
   温度heated
2. 2
   温度at reflux for 5 hours
3. 3
   その他The reaction mixture is evaporated to dryness
4. 4
   その他The crude product is purified by flash chromatography

実験手順

To a solution of 10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (1.66 g, 10 mmol) in chloroform (20 ml) is added PCl5 (1.04 g, 5 mmol) in one portion. The reaction mixture is stirred and heated at reflux for 5 hours. The reaction mixture is evaporated to dryness. The crude product is purified by flash chromatography to give 5-chloro-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (1.29 g).

出典