反应详情

(S)-Benzyl 1-((S)-2-(methoxycarbonylamino)-3-methylbutanoyl)pyrrolidine-2-carboxylate (40 g) and 5% Pd/Alumina were charged to a Parr reactor followed by THF (160 mL). The reactor was sealed and purged with nitrogen (6×20 psig) followed by a hydrogen purge (6×30 psig). The reactor was pressurized to 30 psig with hydrogen and agitated at room temperature for approximately 15 hours. The resulting slurry was filtered through a GF/F filter and concentrated to approximately 135 g solution. Heptane (120 mL) was added, and the solution was stirred until solids formed. After an addition 2-3 hours, additional heptane (240 mL) was added drop-wise, the slurry was stirred for approximately 1 hour, then filtered. The solids were dried to afford the title compound (S)-1-((S)-2-(methoxycarbonylamino)-3-methylbutanoyl)pyrrolidine-2-carboxylic acid.

1. customThe reactor was sealed
2. custompurged with nitrogen (6×20 psig)
3. custompurge (6×30 psig)
4. filtrationThe resulting slurry was filtered through a GF/F
5. filtrationfilter
6. concentrationconcentrated to approximately 135 g solution
7. additionHeptane (120 mL) was added
8. stirringthe solution was stirred until solids
9. customformed
10. additionwas added drop-wise
11. stirringthe slurry was stirred for approximately 1 hour
12. filtrationfiltered
13. customThe solids were dried