反应详情

5-[(cis-4-[4-(7-[2-(Trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]cyclohexylmethyl)thio]-4H-1,2,4-triazol-3-amine (9a) was dissolved in TFA (1 mL) and was stirred for 2 h. The solution was concentrated using a rotary evaporator to remove TFA. The residue was dissolved in methanol (1 mL) and ammonium hydroxide (1 mL) added. The solution was stirred overnight. LCMS showed complete de-protection. The solution was concentrated using a rotary evaporator. The product was isolated by prep LCMS using a 30 mm×100 mm C18 column; 11% CH3CN—H2O (0.1% TFA), 1.5 min, to 33% at 6 min; 60 mL/min; detector set at m/z 396; retention time, 5.5 min (2 runs). The eluate was freeze dried. Yield 21 mg (di-TFA salt). LC/MS (M+H)+: 396,

1. concentrationThe solution was concentrated
2. customa rotary evaporator
3. customto remove TFA
4. dissolutionThe residue was dissolved in methanol (1 mL)
5. additionammonium hydroxide (1 mL) added
6. stirringThe solution was stirred overnight
7. concentrationThe solution was concentrated
8. customa rotary evaporator
9. customThe product was isolated by prep LCMS
10. customretention time, 5.5 min (2 runs)
11. customdried