تفاعل #1054462

ord-8f37cbdff63d4417b78e2802b6931b93

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe product mixture was concentrated
  2. 2
    workup.DISSOLUTIONdissolved in EtOAc (100 mL)
  3. 3
    غسيلwashed twice with 5% aqueous sodium bisulfite (50 mL), twice with saturated aqueous NaHCO3, (50 mL) once with brine (50 mL)
  4. 4
    تجفيفdried with Na2SO4
  5. 5
    تركيزconcentrated

الإجراء التجريبي

A solution of N-trifluoroacetyl-4-chlorophenethylamine (1.6 g, 6.4 mmol) in dichloromethane (20 mL) was treated with bis(pyridine)iodonium(I)tetrafluoroborate (2.6 g, 7.0 mmol), CF3SO3H (2.1 g, 14.1 mmol) and stirred overnight at 20 C. The product mixture was concentrated, dissolved in EtOAc (100 mL), washed twice with 5% aqueous sodium bisulfite (50 mL), twice with saturated aqueous NaHCO3, (50 mL) once with brine (50 mL), dried with Na2SO4 and concentrated to give 0.94 g of a clear oil. MS calculated for C10H8ClF3INO+H: 378, observed: 378.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06953787B2uspto-grants-2005_10