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
4-[2-(4-cyano-3-isoquinolin-4-yl-benzoyl)-3H-imidazo[4,5-b]pyridine-5-yl]piperazine-1-carboxylic acid tert-butyl ester solution (16 mg, 0.029 mmole) in 2 M HCl ethylether (2 ml) was stirred at room temperature for 1 hour. Solvent was removed. Solid was washed with ether for three times and purified by using HPLC (20% to 100% acetonitrile in water with 0.1% NH4OH) to afford product (4.6 mg, 25%) as a yellow solid. 1H NMR (400 MHz, CD2Cl2) δ 2.86 (m, 4H), 3.55 (m, 4H), 6.73 (d, J=9.03 Hz, 1H), 7.59 (d, J=8.03 Hz, 1H), 7.66 (m, 2H), 8.00 (d, J=9.03 Hz, 1H), 7.97 (d, J=8.03 Hz, 1H), 8.07 (d, J=8.03 Hz, 1H), 8.50 (s, 1H), 8.72 (s, 1H), 8.77 (d, J=8.03 Hz, 1H), 9.31 (s, 1H). HR-MS m/z 460.1896 (M+1).
WORKUP
后处理
- customSolvent was removed
- washSolid was washed with ether for three times
- custompurified