反应详情

2′-Acetylamino-4′-methyl-[4,5′]bithiazolyl-2-carbonyl chloride, prepared as in Step I of Example 13, described above (160 mg; 0.53 mmol; 1 eq.), is dissolved in THF (8 ml) and DCM (4 ml). 4-Piperidone hydrochloride monohydrate (Aldrich) (97.7 mg; 0.64 mmol; 1.20 eq.) and triethylamine (0.22 ml; 1.59 mmol; 3 eq.) are added and the mixture is stirred overnight at rt. Solvents are evaporated and the crude product is purified by preparative HPLC, affording Compound (42) as a pale yellow powder (39.2 mg; 20%). 1H NMR (DMSO-d6, 300 MHz) δ 2.14 (s, 3H), 2.49 (s, 3H), 2.53 (m, 4H), 3.94 (m, 2H), 4.53 (m, 2H), 8.03 (s, 1H), 12.17 (s, 1H). M− (ESI): 363.09; M+ (ESI): 365.04. HPLC (method A), Rt: 2.44 min (purity: 95.3%).

1. customSolvents are evaporated
2. customthe crude product is purified by preparative HPLC