Potassium Carbonate → Tert-butyl 2-[(2,2-difluoroethyl)amino]acetate

tert-Butyl bromoacetate (2.72 g) was added to a suspension of 2,2-difluoroethylamine (1.46 g) and potassium carbonate (2.48 g) in acetonitrile (5 mL) and the mixture was stirred at RT for 24 h. The mixture was diluted with EtOAc (10 mL) and hexane (10 mL). The suspension was washed with the mixture of aqueous NaHCO3 (20 mL) and brine (10 mL). The organic extracts were dried and concentrated in vacuo to provide crude product. The crude product was purified by vacuum distillation (12 hPa, 78-80° C.) to afford sub-title compound (1.85 g) as a colourless oil; 1H NMR (300 MHz, CDCl3); 5.82 (1H, tt, J=4.4, 56 Hz), 3.45 (2H, s), 2.98 (2H, dt, J=4.4, 15.1 Hz), 1.45 (9H, s).

1. washThe suspension was washed with the mixture of aqueous NaHCO3 (20 mL) and brine (10 mL)
2. customThe organic extracts were dried
3. concentrationconcentrated in vacuo
4. customto provide crude product
5. distillationThe crude product was purified by vacuum distillation (12 hPa, 78-80° C.)

ORDレコード

ord-f8533fc023044fe58804cd53b4ba5ed8

出典データセット

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09376398B2