反应详情

A solution of 3-[5-(5-chloro-2-methyl-phenyl)-6-(4-chloro-phenyl)-1-isopropyl-4-oxo-1,4,5,6-tetrahydro-pyrrolo[3,4-b]pyrrol-2-yl]-4-methoxy-benzonitrile (Example 17) (0.126 mmol), sodium azide (0.534 mmol) and ammonium chloride (0.534 mmol) in DMF (2 mL) was stirred at 120° C. for 36 h. The mixture was cooled to rt and poured onto ice-H2O and acidified with 1N aqueous HCl. The resulting suspension was filtered. The solid was washed with H2O and dried. The residue was purified by SFC to afford the title compound as a white solid. tR: 4.98 min (HPLC 1); ESI-MS: tR=1.25 min, [M+H]+ 573/575 (LC-MS 1); TLC: Rf=0.21 (9:1 CH2Cl2/MeOH); 1H-NMR (d6-DMSO, 600 MHz): (rotamers) 8.14 (d, 1H), 7.96 (s, 1H), 7.80 (s, 1H), 7.35-7.47 (m, 3H), 7.26 (m, 2H), 7.16 (m, 1H), 7.11 (m, 1H), 6.53 (s, 1H), 6.33 (s, 1H), 3.97 (m, 1H), 3.86 (s, 3H), 1.94 (s, 3H), 1.33 (m, 3H), 0.48 (s, 3H).

1. additionpoured onto ice-H2O
2. filtrationThe resulting suspension was filtered
3. washThe solid was washed with H2O
4. customdried
5. customThe residue was purified by SFC