تفاعل #308465

معادلة التفاعل

N-trifluoroacetyl-4-chlorophenethylamine

bis(pyridine)iodonium(I)tetrafluoroborate

CF3SO3H

→

clear oil

المردود 38.9%

N-Trifluoroacetyl-2-iodo-4-chlorophenethylamine

المردود 38.9%

المذيبات

dichloromethane

ظروف التفاعل

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 to 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 to 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