HRID505554

反应详情

EQUATION

反应方程式

HRID 505554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customthe resulting residue was purified by reverse phase chromatography
  3. washeluting with 30-95% MeCN/H2O+0.1% TFA
  4. concentrationThe product fractions were concentrated under reduced pressure