반응 #564082

ord-903a0d69204941718dd759b1c617b0d2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONWhen the addition
  2. 2
    온도the reaction mixture is heated
  3. 3
    온도under reflux for 5 hours
  4. 4
    기타After return to room temperature, the crystals formed
  5. 5
    여과are filtered off
  6. 6
    세척carefully washed with acetone
  7. 7
    기타dried

실험 절차

40 ml of thionyl chloride are added dropwise to a solution of 60 g of 2-[4-(2,4-difluorophenyl)piperazin-1-yl]ethanol, prepared in Example 2, in 300 ml of chloroform. When the addition is complete, the reaction mixture is heated under reflux for 5 hours. After return to room temperature, the crystals formed are filtered off, carefully washed with acetone and then dried to give 70 g of 1-chloro-2-[4-(2,4-difluorophenyl)piperazin-1-yl]ethane hydrochloride in the form of crystals melting at 218° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04886805uspto-grants-1989_12