Réaction #92114

Équation de réaction

phenyl chloroformate

(3-chloropropyl)(2,2,2-trifluoroethyl)amine

dichloromethane

→

Phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate

Solvants

pyridine

Conditions de réaction

Traitement

1. 1
   AutreInto a 500-mL round-bottom flask, was placed
2. 2
   LavageThe resulting mixture was washed with 2×100 mL of H2O
3. 3
   LavageThe resulting mixture was washed with 2×100 mL of brine
4. 4
   SéchageThe mixture was dried over sodium sulfate
5. 5
   ConcentrationThe resulting mixture was concentrated under vacuum
6. 6
   AutreThis resulted in 1.4 g (crude) of phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate as a colorless liquide

Mode opératoire

Into a 500-mL round-bottom flask, was placed (3-chloropropyl)(2,2,2-trifluoroethyl)amine (5 g, 28.48 mmol, 1.00 equiv), dichloromethane (300 mL), TEA (5.8 g, 57.32 mmol, 2.00 equiv), pyridine (0.5 mL). To this was added dropwise phenyl chloroformate (4.4 g, 28.10 mmol, 1.00 equiv) at 0° C. The resulting solution was stirred for 3 h at room temperature. The resulting mixture was washed with 2×100 mL of H2O. The resulting mixture was washed with 2×100 mL of brine. The mixture was dried over sodium sulfate. The resulting mixture was concentrated under vacuum. This resulted in 1.4 g (crude) of phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate as a colorless liquide.

Source