Sodium Hydroxide → 5,5,5-Trifluoro-3-(2,2,2-trifluoroethyl)-DL-norvaline

5-(3,3,3-Trifluoro-1-(2,2,2-trifluoroethyl)propyl)imidazolidine-2,4-dione (1.0 g, 3.59 mmol) was dissolved in a 10 mL solution of aqueous NaOH (0.575 g in 10 mL H2O, 14.38 mmol). The solution was divided in 2 special vessels for microwave technology. The solution was heated by microwave in sealed vessels for 1 h. Microwave conditions: 15 min at about 100% power, 150° C., 50 psi, then 5 min at rest, 0% power. The sequence was repeated until the reaction was done. Water and ammonia were removed from the reaction mixture in vacuo and the resulting crude 5,5,5-trifluoro-3-(2,2,2-trifluoroethyl)-dl-norvaline (0.92 g, 100%) and NaOH mixture was used in the next reaction without further purification. Mass Spectrum (+ESI): 254 (M+H)+.

1. temperatureThe solution was heated by microwave in sealed vessels for 1 h
2. custom15 min
3. customat about 100% power, 150° C., 50 psi
4. custom5 min
5. customWater and ammonia were removed from the reaction mixture in vacuo
6. customthe resulting crude 5,5,5-trifluoro-3-(2,2,2-trifluoroethyl)-dl-norvaline (0.92 g, 100%) and NaOH mixture was used in the next reaction without further purification

ORD record

ord-26191dc0fff94ea9854a4d3aa7a6f4a3

Source dataset

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07547725B2