反応 #69971

反応方程式

4-bromophenylpiperazine

triethylamine

benzyl chloroformate

→

4-(4-bromophenyl)piperazine-1-carboxylic acid benzyl ester

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度The mixture is cooled in an ice bath
2. 2
   その他to return to ambient temperature
3. 3
   その他gentle hydrolysis
4. 4
   抽出The aqueous phase is extracted with dichloromethane
5. 5
   洗浄washed with a saturated NaCl solution
6. 6
   乾燥dried over sodium sulphate
7. 7
   ろ過filtered through a sintered glass
8. 8
   ろ過filter
9. 9
   濃縮concentrated under vacuum

実験手順

5 g of 4-bromophenylpiperazine are placed in a 500 ml three-necked flask under a nitrogen atmosphere. 4.34 ml of triethylamine are added. The mixture is cooled in an ice bath and 3.24 ml of benzyl chloroformate are added. The mixture is allowed to return to ambient temperature. It is diluted with dichloromethane and then gentle hydrolysis is carried out. The aqueous phase is extracted with dichloromethane. The organic phases are combined, washed with a saturated NaCl solution, dried over sodium sulphate, then filtered through a sintered glass filter and concentrated under vacuum. 8.43 g of 4-(4-bromophenyl)piperazine-1-carboxylic acid benzyl ester are obtained.

出典