HRID655837

反应详情

EQUATION

反应方程式

HRID 655837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Title compound 10A, 1-(4-nitro-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (1.0 g, 3.9 mmol) was added to 10% w/w palladium on carbon (0.1 g, 10% w/w) suspended in ethanol (300 ml). This was stirred for 42 hours at room temperature under an atmosphere of hydrogen. The reaction mixture was filtered to remove the palladium residues and the filtrate was concentrated to dryness in vacuo. The resultant residue was purified by column chromatography using DCM/MeOH (96:4) as eluent to yield the title compound as an off-white solid. (0.53 g, 2.3 mmol, 60%). LCMS: [M+H]+=227, Rt=0.64 min, 100% purity.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customto remove the palladium residues
  3. concentrationthe filtrate was concentrated to dryness in vacuo
  4. customThe resultant residue was purified by column chromatography