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 solution of tert-butyl 4-hydroxy-4-(6-(6-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)azepane-1-carboxylate (200 mg, 0.41 mmol) in a solution of HCl in MeOH (2.0 M, 10 mL) was stirred at room temperature for 1 hour, which was monitored by LCMS. After completion of the reaction, the reaction mixture was concentrated under reduced pressure. The crude was purified by reverse phase preparative HPLC to afford 230 as a light yellow solid (30 mg, 31%). 1H NMR (500 MHz, CDCl3) δ (ppm) 9.06 (s, 1H), 8.85 (s, 1H), 8.26 (s, 1H), 8.06 (s, 1H), 8.03 (s, 1H), 7.88-7.89 (d, J=4.5 Hz, 2H), 7.56-7.58 (t, J=9 Hz, 1H), 4.00 (s, 3H), 3.31-3.38 (m, 2H), 3.10-3.13 (t, J=13 Hz, 1H), 2.81-2.83 (t, J=12 Hz, 1H), 2.37-2.46 (m, 3H), 2.10-2.17 (m, 4H), 1.82-1.85 (t, J=14.5 Hz, 1H); MS (ESI) m/z: 390 [M+H]+.
WORKUP
后处理
- customAfter completion of the reaction
- concentrationthe reaction mixture was concentrated under reduced pressure
- customThe crude was purified by reverse phase preparative HPLC