HRID339010

反应详情

EQUATION

反应方程式

HRID 339010 的结构方程式

PROCEDURE

实验过程

To a solution of tert-butyl (S)-1-((R)-1-(3-(8-((R)-1-(tert-butyldimethylsilyloxy)propan-2-yloxy)quinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)-2,2,2-trifluoroethyl)pyrrolidin-3-ylcarbamate (0.29 g, 0.41 mmol) in dichloromethane (1 mL) was added trifluoroacetic acid (2 mL) was stirred at ambient temperature for 30 minutes. The reaction mixture was concentrated under reduced pressure. The residue was purified by reverse phase chromatography on C18 (0-80% acetonitrile/water). The material isolated after purification was dissolved in methanol (0.5 mL) and added dropwise to hydrochloric acid (2M in diethyl ether; 5 mL). The resulting salt was collected by vacuum filtration to provide the title compound (0.17 g, 73%). LCMS APCI (+) m/z 487 (M+H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customThe residue was purified by reverse phase chromatography on C18 (0-80% acetonitrile/water)
  3. customThe material isolated
  4. customafter purification
  5. dissolutionwas dissolved in methanol (0.5 mL)
  6. additionadded dropwise to hydrochloric acid (2M in diethyl ether; 5 mL)
  7. filtrationThe resulting salt was collected by vacuum filtration