HRID556830

反应详情

EQUATION

反应方程式

HRID 556830 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-(3-(2-(tert-butyldimethylsilyloxy)ethylcarbamoyl)-1H-pyrrol-1-yl)-2-(5-cyanopyrazin-2-ylamino)pyridin-4-ylamino)methyl)piperidine-1-carboxylate (80 mg, 0.118 mmol) was dissolved in THF (2 mL) and tetrabutylammonium fluoride on silica (1.5 mmol/g; 237 mg, 0.355 mmol) was added. The reaction mixture was stirred for 1 h at room temperature. The mixture was filtered and the solvent was evaporated. The residue was dissolved in methanol (1 mL) and absorbed on to a TsOH solidphase extraction cartridge. After 1.5 h the cartridge was eluted with 7M ammonia in methanol. The eluent was evaporated to dryness and the residue was purified by HPLC to give 1-(6-(5-cyanopyrazin-2-ylamino)-4-(piperidin-3-ylmethylamino)pyridin-3-yl)-N-(2-hydroxyethyl)-1H-pyrrole-3-carboxamide.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in methanol (1 mL)
  4. customabsorbed on to a TsOH solidphase extraction cartridge
  5. washAfter 1.5 h the cartridge was eluted with 7M ammonia in methanol
  6. customThe eluent was evaporated to dryness
  7. customthe residue was purified by HPLC