تفاعل #51769

ord-5fa63e22d0ae4f559d38c467eb838e0c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىHCl gas was bubbled through the solution for 15 minutes
  2. 2
    أخرىThe solvents were evaporated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in MeOH (10 mL)
  4. 4
    workup.ADDITIONtreated with pH 7.5 buffer
  5. 5
    أخرىThe precipitate that formed
  6. 6
    ترشيحwas filtered
  7. 7
    أخرىdried

الإجراء التجريبي

Toluene-4-thiosulfonic acid S-(4,5-bis-tert-butoxycarbonylamino-2-isopropyl-phenyl)ester (prepared in Example UU-1; 8.88 g, 16.6 mmol) was dissolved in CH2Cl2 (25 mL), and HCl gas was bubbled through the solution for 15 minutes. The reaction mixture was stirred at room temperature for 90 minutes. The solvents were evaporated, and the residue was dissolved in MeOH (10 mL) and treated with pH 7.5 buffer. The precipitate that formed was filtered and dried. MS(APCI): 337 (M+H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06852711B2uspto-grants-2005_02