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
8-(2-Fluoro-4-iodo-phenylamino)-imidazo[1,5-a]pyridine-7-carboxylic acid (2-vinyloxy-ethoxy)-amide (151 mg, 0.31 mmol) was dissolved in methanol and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was then washed with methanol and the desired product was subsequently eluted using 2M NH3 in MeOH. Appropriate fractions were combined and concentrated to give a residue that was subjected to flash chromatography (Si-PPC, gradient 0% to 10%, methanol in dichloromethane) to afford the title compound as a pale yellow solid (115 mg, 81%). LCMS (method A): RT=6.36 min, [M+H]+=457. 1H NMR (CD3OD): 8.27 (1H, d, J=0.85 Hz), 7.80-7.77 (1H, m), 7.57-7.53 (1H, m), 7.49-7.46 (1H, m), 6.95 (1H, t, J=8.48 Hz), 6.76 (1 H, d, J=7.37 Hz), 6.68 (1H, s), 4.00-3.94 (2 H, m), 3.75-3.71 (2 H, m).
WORKUP
后处理
- washThe cartridge was then washed with methanol
- washthe desired product was subsequently eluted
- concentrationconcentrated
- customto give a residue that