反应详情

温度

60 °C

The crude (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-[(1-methylethyl)amino]butanoic acid hydrochloride was dissolved in MeCN (20 mL) and treated with HMDS (4 mL) and the reaction was stirred at 60° C. for 15 h. After cooled down, the reaction was diluted with H2O and extracted with Et2O (2×). The combined organic extracts were washed with H2O (2×), dried over Na2SO4, filtered, concentrated, and purified by silica gel chromatography with 25% EtOAC in hexane grading to 100% EtOAc in hexane to yield the titled product (0.13 g, 49%). LC-MS (ES) m/e 277.9 (M+H)+.

1. temperatureAfter cooled down
2. extractionextracted with Et2O (2×)
3. washThe combined organic extracts were washed with H2O (2×)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by silica gel chromatography with 25% EtOAC in hexane grading to 100% EtOAc in hexane