反応 #92114

反応方程式

phenyl chloroformate

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

dichloromethane

→

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

溶媒

pyridine

反応条件

後処理

1. 1
   その他Into a 500-mL round-bottom flask, was placed
2. 2
   洗浄The resulting mixture was washed with 2×100 mL of H2O
3. 3
   洗浄The resulting mixture was washed with 2×100 mL of brine
4. 4
   乾燥The mixture was dried over sodium sulfate
5. 5
   濃縮The resulting mixture was concentrated under vacuum
6. 6
   その他This resulted in 1.4 g (crude) of phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate as a colorless liquide

実験手順

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.

出典