HRID2368181

反应详情

EQUATION

反应方程式

HRID 2368181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2,2-Trifluoroacetic acid (0.283 mL, 3.68 mmol) was added to a solution of N-(3-(6-((3-fluoro-4-morpholinophenyl)amino)-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl)phenyl)acrylamide (20 mg, 0.037 mmol) in CH2Cl2 (5 mL), and the reaction mixture was stirred overnight at room temperature, after which the solvent was removed by vacuum. The residue was purified by flash column chromatography (5% CH3OH/CH2Cl2) to yield the title compound as a solid. 1H NMR (400 MHz, CD3OD): δ 8.72 (s, 1H), 8.34 (s, 1H), 8.01 (d, 1H, J=8.4 Hz), 7.94 (m, 1H), 7.73 (m, 1H), 7.54 (t, 1H, J=8.0 Hz), 7.41 (m, 1H), 7.01 (t, 1H, J=9.6 Hz), 6.44 (m, 2H), 5.81 (dd, 1H, J=2.4 & 9.6 Hz), 3.85 (m, 4H), 3.05 (m, 4H); ESI-MS: [M+H]+.

WORKUP

后处理

  1. customafter which the solvent was removed by vacuum
  2. customThe residue was purified by flash column chromatography (5% CH3OH/CH2Cl2)