반응 #52195

ord-789b1999ccb742508406e6b1f8486403

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After the mixture was filtered
  2. 2
    workup.DISSOLUTIONthe resulting solid was dissolved in 5 ml dioxane
  3. 3
    여과Solid was filtered
  4. 4
    세척washed with water
  5. 5
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855720B2uspto-grants-2005_02