反应详情

温度

0 °C

1-(2-Hydroxy-2-phenyl-3,3,3-trifluoropropanoyl)-N-(2-tert-butyloxycarbonylaminomethyl-5-chlorobenzyl)-L-prolinamide from step 3 (more polar isomer, 8.5 mg, 0.015 mmol) was dissolved in EtOAc (20 mL) and cooled with stirring to 0° C. Into this solution was bubbled in HCl gas for 5 min. The resulting solution was stirred at 0° C. for 30 min. The hydrochloride salt of the title compound was obtained as a white crystalline solid after concentrating the reaction in vacuo (HPLC RT=2.78 min, method A; LC-MS m/z=470.1; 1H NMR, 400 MHz, CD3OD, 7.54 ppm (m, 3H), 7.44 ppm (d, 1H), 7.42 ppm (m, 1H), 4.5 ppm (d, 1H), 4.4 ppm (m, 2H), 4.3 ppm (m, 2H), 3.75 ppm (m, 1H), 2.7 pm (m, 1H), 2.1 ppm (m, 1H), 1.7 ppm (m, 3H)).

1. temperaturecooled
2. customInto this solution was bubbled in HCl gas for 5 min
3. stirringThe resulting solution was stirred at 0° C. for 30 min