反应详情

Cbz-protected amine 14 (107 mg, 0.23 mmol) was dissolved in MeOH (5 mL) and to this was added TFA (1.2 eq., 0.27 mmol, 21 μL). Argon was bubbled through the solution for 15 minutes, after which Pd black (10 mg) was added and the flask was charged with hydrogen gas. After 10 minutes, TLC analysis indicated complete conversion of starting material and all solids were removed by filtration over CELITE. Toluene (10 mL) was added and the mixture was concentrated under reduced pressure followed by coevaporation with toluene (2×) in order to remove excess TFA. The purity of the deprotected amine (as TFA salt) was confirmed by LC-MS analysis and the compound was subjected to the next step without further purification.

1. customArgon was bubbled through the solution for 15 minutes
2. additionafter which Pd black (10 mg) was added
3. additionthe flask was charged with hydrogen gas
4. customall solids were removed by filtration over CELITE
5. additionToluene (10 mL) was added
6. concentrationthe mixture was concentrated under reduced pressure
7. customto remove excess TFA
8. customthe compound was subjected to the next step without further purification