反応 #72718

反応方程式

22

4-Benzylidene-2-(2-chloro-phenyl)-4H-oxazol-5-one

AlCl3

→

desired product

収率 35.0%

1-(2-Chloro-phenyl)-isoquinoline-3-carboxylic acid

収率 35.0%

溶媒

tetrachloroethane

tetrachloroethane

反応条件

後処理

1. 1
   その他The reaction mixture was quenched by addition of 1 M HCl (50 ml)
2. 2
   workup.ADDITIONThen, the mixture was basified by addition of NaOH (1M aqueous solution)
3. 3
   その他the resulted layers were separated
4. 4
   抽出This aqueous phase was extracted with CH2Cl2
5. 5
   乾燥dried over MgSO4
6. 6
   その他finally the solvents were removed under reduced pressure

実験手順

A solution of 22 (12 mmol) in tetrachloroethane was added to the suspension of AlCl3 (36 mmol) in tetrachloroethane (50 ml). The resulting mixture was heated to 60° C. for 1.5 hrs. The reaction mixture was quenched by addition of 1 M HCl (50 ml). Then, the mixture was basified by addition of NaOH (1M aqueous solution), the resulted layers were separated, and the aqueous layer was acidified by HCl (aqueous solution). This aqueous phase was extracted with CH2Cl2, dried over MgSO4 and finally the solvents were removed under reduced pressure, to give 35% yield of the desired product.

出典