تفاعل #5826

ord-5e959f0c247e4beda9969377311282aa

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction mixture was stirred for 16 hours
  2. 2
    أخرىThe reaction mixture was evaporated
  3. 3
    أخرىto remove the solvent under a reduced pressure
  4. 4
    workup.ADDITIONto the residue was added benzene, and insoluble matter
  5. 5
    ترشيحwas filtered by suction
  6. 6
    غسيلwashed with benzene
  7. 7
    أخرىevaporated off under a reduced pressure
  8. 8
    غسيلeluted with chloroform/methanol (100:1)

الإجراء التجريبي

15.29 g of N-tert-butoxycarbonyltyrosine and 12.73 g of N-benzyloxycarbonylhomopiperazine were dissolved in 280 ml of tetrahydrofuran, to the solution were added 8.09 g of 1-hydroxybenzotriazole hydrate and 11.77 g of DCC at a room temperature with stirring, and the reaction mixture was stirred for 16 hours. The reaction mixture was evaporated to remove the solvent under a reduced pressure, to the residue was added benzene, and insoluble matter was filtered by suction and washed with benzene. The benzene layers were combined and evaporated off under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (100:1), to obtain 26.42 g of the title compound in colorless amorphous form.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05245034uspto-grants-1993_09