HRID1887309
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of N-benzyl-2-(3-(benzyloxy)-2-oxopyridin-1(2H)-yl)-4-methylthiazole-5-carboxamide (0.14 g, 0.32 mmol) and 20 wt. % palladium on activated carbon (0.10 g) in methanol (50 mL) was stirred under an atmosphere of hydrogen for 2 hours. The mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography followed by recrystallization from methanol (10 mL) to afford the title compound (0.027 g, 8%): mp 225-228° C.; 1H NMR (300 MHz, CD3OD) δ 8.63 (d, J=7.6 Hz, 1H), 7.42-7.26 (m, 5H), 6.20-6.10 (m, 1H), 5.87-5.83 (m, 1H), 4.36 (d, J=6.0 Hz, 2H), 2.58 (s, 3H); MS (ES+) m/z 342.2 (M+1).
WORKUP
后处理
- filtrationThe mixture was filtered
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by column chromatography
- customfollowed by recrystallization from methanol (10 mL)