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

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.

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

ORD record

ord-d88794e752b94b8592b3cde2735736e0

Source dataset

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09447084B2