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 {3,5-dichloro-4-[4-(6-methylpyrimidin-4-ylamino)thiazolo[5,4-c]pyridin-2-yl]-phenyl}-carbamic acid tert-butyl ester (235 mg, 0.467 mmol) in 4N HCl in dioxane (10 mL) was heated at 50° C. for 3 hours under a nitrogen atmosphere. After cooling to room temperature, the reaction mixture was filtered and the precipitate collected. The solid thus obtained was purified by column chromatography on silica gel eluting with 0-5% 2N NH3/MeOH in EtOAc to afford the title compound as a pale yellow solid (142 mg, 75% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.54 (s, 1H), 8.62 (d, J=1.2 Hz, 1H), 8.41 (d, J=5.6 Hz, 1H), 7.77 (d, J=5.6 Hz, 1H), 7.63 (s, 1H), 6.77 (s, 2H), 6.22 (s, 2H), 2.39 (s, 3H). LCMS (Method C): RT=2.97 min, m/z: 403 [M+H+].
WORKUP
后处理
- filtrationthe reaction mixture was filtered
- customthe precipitate collected
- customThe solid thus obtained
- customwas purified by column chromatography on silica gel eluting with 0-5% 2N NH3/MeOH in EtOAc