HRID1398597
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
To a solution of 1-(2-aminopyrimidin-4-yl)-N,N-dimethyl-6-[2-(trimethylsilyl)ethynyl]indazole-3-carboxamide (250 mg, 0.66 mmol) in methanol (5 mL) and DCM (10 mL) was added K2CO3(182.57 mg, 1.32 mmol). The reaction mixture was stirred for 1 hr and then filtered by suction filtration. The precipitate was washed with DCM and methanol and the filtrate was concentrated in vacuo to give the title intermediate: 1H NMR (250 MHz, DMSO) delta 3.08 (3H, s), 3.29 (3H, br. s.), 4.42 (1H, s), 7.06 (1H, d, J=5.63 Hz), 7.14 (2H, br. s.), 7.41-7.48 (1H, m), 7.97 (1H, d, J=8.22 Hz), 8.31 (1H, d, J=5.48 Hz), 9.04 (1H, s); LC-MS: m/z=+307.00 (M+H)+.
WORKUP
后处理
- filtrationfiltered by suction filtration
- washThe precipitate was washed with DCM and methanol
- concentrationthe filtrate was concentrated in vacuo