反应详情

To a solution of 2-bromo- 1-[4-methyl-2-(pyrazin-2-ylamino)-1,3 -thiazol-5-yl]lethanone, (Intermediate 3) (75 mg; 0.19 mmol; 1 eq.) in EtOH (2 ml), is added triethylamine (66 μl; 0.48 mmol; 2.50 eq.) and 2-cyanothioacetamide (19.0 mg; 0.19 mmol; 1 eq.). The mixture is stirred overnight at rt. The reaction mixture is filtered and rinsed -with ethanol affording Compound (53) as brown solid (35.4 mg; 59%). 1H NMR (DMSO-d6) δ2.49 (s, 3H), 4.62 (s, 2H), 7.67 (s, 1H), 8.13 (m, 1H), 8.36 (m, 1H), 8.44 (m, 1H), 11.79 (br s, 1H). M31 (ESI): 312.88; M+(ESI): 314.95. HPLC (method A), Rt: 2.47 min (purity: 93.5%).

1. filtrationThe reaction mixture is filtered
2. washrinsed -with ethanol affording Compound (53) as brown solid (35.4 mg; 59%)