反应详情

温度

0 °C

Dissolve (R)-1-methyl-2,2,2-trifluoroethylamine hydrochloride (3.73 g, 25 mmol) in chloroform (50 mL) containing triethylamine (3.5 mL, 25 mmol). Cool to 0° C. in an ice bath and dropwise add benzoyl isothiocyanate (3.35 mL, 25 mmol) over 10 min. Warm the mixture to room temperature and stir overnight. Concentrate in vacuo and purify by chromatography on silica gel (200 g) eluting with hexane/EtOAc (19:1 to 4:1 over 40 min; 50 mL/min) to afford the desired intermediate as a light yellow oil (6.2 g, 90%).

1. temperatureWarm the mixture to room temperature
2. concentrationConcentrate in vacuo
3. custompurify by chromatography on silica gel (200 g)
4. washeluting with hexane/EtOAc (19:1 to 4:1 over 40 min; 50 mL/min)