反応 #52195

反応方程式

1-(3-trifluoromethylphenyl)piperazine

ethyl 3-bromopropionate

sodium bicarbonate

→

3-[4-(3-trifluoromethylphenyl)-1-piperazinyl]propionic acid

収率 75.2%

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過After the mixture was filtered
2. 2
   workup.DISSOLUTIONthe resulting solid was dissolved in 5 ml dioxane
3. 3
   ろ過Solid was filtered
4. 4
   洗浄washed with water
5. 5
   その他dried

実験手順

The reaction mixture of 1-(3-trifluoromethylphenyl)piperazine (510 mg, 2.2 mmol), ethyl 3-bromopropionate (500 mg, 2.7 mmol), sodium bicarbonate (300 mg, 3.5 mmol) and ethanol (15 ml) was refluxed for 3 h till the amine disappeared completely. After the mixture was filtered, the resulting solid was dissolved in 5 ml dioxane and 14 ml 5% sodium hydroxide solution. The mixture was stirred at room temperature overnight, then it was acidified with concentrated hydrogen chloride. Solid was filtered and washed with water, and then dried to give 500 mg 3-[4-(3-trifluoromethylphenyl)-1-piperazinyl]propionic acid as a white solid, mp 228-230° C.

出典