反应详情

To a 500 mL four-neck round bottom flask, 34.0 g (R)-N-benzyl-2-(tert-butoxycarbonylamino)-3-hydroxypropionamide and 350 mL dichloromethane were added, and the mixture was stirred to obtain a clear solution. At 20-25° C., 40.0 g concentrated hydrochloric acid (having a mass concentration of 36.0%) was added, and the reaction was continued. TLC tracking was performed, till the raw materials were completely converted. After the reaction was completed, the temperature was decreased to 20° C. The mixture was suction-filtered, to obtain a white needle-like crystal. The obtained white crystalline solid was dissolved in 50 g water. At 20-25° C., 30% sodium hydroxide solution was added to adjust the pH value of the system to 8-9. After the addition, the solution was stirred continuously, and a white flaky crystal was precipitated. The mixture was suction-filtered, and the filter was washed and dried, to obtain a target product of 16.5 g (0.085 mol). The molar yield was 73.52%.

1. customto obtain a clear solution
2. customAt 20-25° C.
3. additionwas added
4. customwas decreased to 20° C
5. filtrationThe mixture was suction-filtered
6. customto obtain a white needle-like crystal
7. additionAfter the addition
8. stirringthe solution was stirred continuously
9. customa white flaky crystal was precipitated
10. filtrationThe mixture was suction-filtered
11. washthe filter was washed
12. customdried
13. customto obtain a target product of 16.5 g (0.085 mol)