反応 #69945

反応方程式

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

PCl5

→

5-chloro-1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one

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 The crude product
4. 4
   その他is purified by flash chromatography on silica gel

実験手順

To a solution of 1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (3 g, 16.6 mmol) in chloroform (8 ml) is added PCl5 portionwise. 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 on silica gel to give 5-chloro-1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (1.39 g).

出典