Reacción #524501

Ecuación de reacción

difluorocaprolactam

ε-Aminocaprolactam

Fluoroxytrifluoromethane

trifluoro-caprolactam

→

Fluoro-ε-aminocaprolactam

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroAfter 11/2 hours more ultraviolet irradiation under similar conditions
2. 2
   Otrothe solvent is removed by distillation
3. 3
   OtroThe residue is quenched with ice and water
4. 4
   Extracciónextracted 3 times with ethyl acetate
5. 5
   LavadoThe combined extracts are washed with aqueous sodium bicarbonate solution
6. 6
   Secadodried over magnesium sulfate
7. 7
   Otroevaporated to dryness
8. 8
   Otroto give

Procedimiento

ε-Aminocaprolactam (2.26 g., 0.02 mole) is dissolved in 60 ml. of liquid HF. Fluoroxytrifluoromethane (10.4 g., 0.1 mole) is passed into the solution under ultraviolet irradiation over 51/2 hours, while kept under vigorous stirring in a dry-ice-acetone cooling bath. After 11/2 hours more ultraviolet irradiation under similar conditions, the solvent is removed by distillation. The residue is quenched with ice and water and extracted 3 times with ethyl acetate. The combined extracts are washed with aqueous sodium bicarbonate solution, dried over magnesium sulfate and evaporated to dryness, to give a mixture of C-fluorinated caprolactams, with the main components being difluorocaprolactam and trifluoro-caprolactam.

Fuente