HRID2067013

反应详情

EQUATION

反应方程式

HRID 2067013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8-(4-Cyclopropyl-2-fluoro-phenylamino)-imidazo[1,5-a]pyridine-7-carboxylic acid (2-vinyloxy-ethoxy)-amide (56 mg, 0.14 mmol) was dissolved in methanol and loaded onto an Isolute® SCX-2 cartridge (5 g). The cartridge was then washed with methanol and the desired product was subsequently eluted using 2M NH3 in MeOH. The eluent was collected and concentrated to give a residue. The residue was subjected to flash chromatography (Si-PPC, gradient 0% to 20%, methanol in dichloromethane) to afford the title compound as a pale yellow solid (37 mg, 71%). LCMS (method A): RT=6.40 min, [M+H]+=371. 1H NMR (CH3OH-d4): 8.20 (1 H, d, J=0.71 Hz), 7.67-7.65 (1 H, m), 7.17-7.11 (1 H, m), 6.94-6.87 (2H, m), 6.73 (1 H, d, J=7.38 Hz), 6.39 (1 H, s), 4.00-3.97 (2 H, m), 3.75-3.72 (2 H, m), 1.98-1.89 (1 H, m), 1.04-0.98 (2 H, m), 0.73-0.68 (2 H, m).

WORKUP

后处理

  1. washThe cartridge was then washed with methanol
  2. washthe desired product was subsequently eluted
  3. customThe eluent was collected
  4. concentrationconcentrated
  5. customto give a residue