反应详情

A solution of biphenyl azido-Thr methyl ester (6) (244 mg, 0.67 mmol) in MeOH (10 ml) was made by sonicating until the milky precipitate cleared. After bubbling nitrogen through the reaction solution for 30 sec., 10% Pd/C was added in one portion. The reaction was stirred under nitrogen at RT. The reaction was exposed to aspirator vacuum to remove the nitrogen and then opened to the hydrogen gas at balloon pressure (˜1 atm). The reaction stirred for 3 h at which time the hydrogen was exchanged for nitrogen. The reaction was filtered through a pad of celite to remove the palladium. The celite pad was washed with MeOH (30 ml). The combined fractions of MeOH were evaporated under reduced pressure and dried in vacuo to give 225 mg (99% yield) of pure produce (7) as a white solid.

1. customby sonicating until the milky precipitate
2. customAfter bubbling nitrogen through the reaction solution for 30 sec
3. addition, 10% Pd/C was added in one portion
4. customto remove the nitrogen
5. stirringThe reaction stirred for 3 h at which time the hydrogen
6. filtrationThe reaction was filtered through a pad of celite
7. customto remove the palladium
8. washThe celite pad was washed with MeOH (30 ml)
9. customThe combined fractions of MeOH were evaporated under reduced pressure
10. customdried in vacuo
11. customto give 225 mg (99% yield)