反应详情

To a 25 mL pear flask was added tert-butyl ((S)-1-(5-((S)-1-((2-amino-5-cyano-6-methylpyrimidin-4-yl)amino)ethyl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-6-yl)pyrrolidin-3-yl)(methyl)carbamate (61 mg, 0.121 mmol) in dichloromethane (0.8 mL) to give a solution. To this solution was added TFA (0.27 mL), and the mixture was stirred at room temperature for 18 hours. All the volatiles were removed in vacuo, and the residue was re-suspended in toluene and concentrated to remove residual TFA. The residue was then diluted in ACN and water (total of about 90 mL), followed by the addition of 2 N HCl (4 mL). The mixture was then lyophilized to give an HCl salt of the title compound as a yellow-green solid (41 mg, 84%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.66 (d, J=6.82 Hz, 2H), 2.17 (td, J=12.69, 7.20 Hz, 1H), 2.31-2.45 (m, 3H), 2.61 (s, 2H), 3.20-3.39 (m, 2H), 3.46 (br s, 1H), 3.57 (br s, 1H), 3.95 (s, 3H), 5.91 (t, J=6.95 Hz, 1H), 6.79 (br s, 1H), 7.68 (br s, 1H), 8.03 (br s, 1H), 8.48 (br s, 1H), 8.77 (br s, 1H), 9.32-9.50 (m, 1H), 9.60-9.82 (m, 1H); ESI-MS m/z [M+H]+ calc'd for C21H27N9, 406. found 406.

1. customto give a solution
2. customAll the volatiles were removed in vacuo
3. concentrationconcentrated
4. customto remove residual TFA
5. additionThe residue was then diluted in ACN
6. additionwater (total of about 90 mL), followed by the addition of 2 N HCl (4 mL)