Tert-Butylamine → 2,2,2-Trifluoroethane-1-sulfonamide

Tetrahydrofuran (6 mL) was added to tert-butylamine (220 mg, 3.0 mmol), and 2,2,2-trifluoroethanesulfonyl chloride (300 mg, 1.6 mmol) was slowly added dropwise thereto. The mixture was stirred at room temperature for 30 minutes, and the solvent was evaporated off under reduced pressure. To the residue, trifluoroacetic acid (3.3 mL) was added and the mixture was stirred at room temperature for 15 hours. The solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=100/0 to 5/1) was performed to give 2,2,2-trifluoroethanesulfonamide (Compound GC) (66 mg, yield: 25%).

1. additionwas slowly added dropwise
2. customthe solvent was evaporated off under reduced pressure
3. additionTo the residue, trifluoroacetic acid (3.3 mL) was added
4. stirringthe mixture was stirred at room temperature for 15 hours
5. customThe solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=100/0 to 5/1)

ORD record

ord-f51f5d34c54742c5b261a348096b4291

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08673908B2