Acetyl chloride → HCID 71571780, compound

Participants

Reaction Steps

To a mixture of N-(3-chloro-4-fluorophenyl)-6-(3-(hexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)propoxy)-7-methoxyquinazolin-4-amine (0.10 g) and Et3N (0.072 g) at 0° C. was added acetyl chloride (0.019 g) dropwise and the reaction was continued to stir for 2 h at same temperature. Then the mixture was diluted with water and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4 and filtered. The solvent of the filtrate was removed by reduce vacuum pressure, and the residue was recrystallized from DCM/PE to give the title compound (0.04 g, 40.00%), HPLC: 96.24%. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 514.2 (M+1); 1H NMR (400 MHz, CDCl3) δ: 1.50-1.53 (m, 2H), 1.83-1.87 (m, 2H), 2.25-2.29 (m, 3H), 2.30 (s, 3H), 2.44 (t, J=4.2 Hz, 2H), 2.90-2.93 (m, 1H), 3.50-3.61 (m, 4H), 4.03 (s, 3H), 4.08 (t, J=4.8 Hz, 2H), 7.16 (s, 1H), 7.26 (s, 1H), 7.45 (s, 1H), 7.57-7.60 (m, 1H), 7.91-7.95 (m, 1H), 8.64 (s, 1H) ppm.

Provenance & Evidence