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
tert-butyl 3-{[5-chloro-4-(2,5-dichloro-3-cyanophenoxy)-2H-1,2,3-benzotriazol-2-yl]methyl}-1H-pyrazolo[3,4-b]pyridine-1-carboxylate (100 mg, 0.175 mmol) was dissolved in TFA (5 mL) at room temperature. After 20 minutes, the reaction mixture was concentrated under reduced pressure, and the resulting residue was purified by reverse phase chromatography eluting with 30-95% MeCN/H2O+0.1% TFA. The product fractions were concentrated under reduced pressure to yield the title compound. 1H NMR (DMSO-d6) δ 13.80 (s, 1H), 8.44 (d, J=2.9 Hz, 1H), 7.99 (d, J=2.2 Hz), 7.95 (m, 1H), 7.93 (d, J=9.2 Hz, 1H), 7.62 (d, J=9.2 Hz, 1H), 7.35 (d, J=2.3 Hz, 1H), 7.16 (dd, J=8.0 Hz, J=4.6 Hz, 1H), 6.30 (s, 2H). HRMS (M+1)=470.0076.
WORKUP
后处理
- concentrationthe reaction mixture was concentrated under reduced pressure
- customthe resulting residue was purified by reverse phase chromatography
- washeluting with 30-95% MeCN/H2O+0.1% TFA
- concentrationThe product fractions were concentrated under reduced pressure