反应详情

温度

70 °C

tert-Butyl (1S,2R)-2-(6-(2,4-dimethoxybenzyl)-4-(1-methyl-1H-pyrazol-4-yl)-5-oxo-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-ylamino)cyclohexylcarbamate (0.0625 g, 0.108 mmol) was dissolved in TFA (2 mL) and heated at 70° C. for 1 h. The solvent was removed under reduced pressure and the resulting residue was dispersed in DMSO/MeOH (1/1) solution. A pale purple precipitate was formed and was separated by filtration. The filtrate, which contained the product, was purified via reverse phase preparative HPLC. Lyophilized fractions gave a TFA salt of the title compound as a white solid (21 mg, 59%). 1H NMR (500 MHz, DMSO-d6) δ ppm 1.28-1.52 (m, 2 H) 1.51-1.94 (m, 6 H) 3.93 (s, 3 H) 4.14-4.30 (m, 2 H) 4.29-4.58 (m, 1 H) 7.51 (d, J=6.83 Hz, 1 H) 7.71 (br s, 2 H) 8.29 (s, 1 H) 8.34-8.69 (m, 1 H) 9.11 (d, J=17.09 Hz, 1 H). [M+H] calc'd for C16H21N7O, 328; found, 328.

1. customThe solvent was removed under reduced pressure
2. additionthe resulting residue was dispersed in DMSO/MeOH (1/1) solution
3. customA pale purple precipitate was formed
4. customwas separated by filtration
5. customwas purified via reverse phase preparative HPLC