HRID1809727

反应详情

EQUATION

反应方程式

HRID 1809727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of (2-morpholin-4-yl-ethyl)-[3-{3-[(thiophen-2-ylmethyl)-amino]-phenyl}-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-amine (170 mg, 0.3 mmol) in dichloromethane (10 mL) was added TFA (10 mL) at room temperature. The resulting mixture was stirred for another three hours at this temperature. The solvent was evaporated under reduced pressure and the residue was dissolved in EtOAc (10 mL). The organic phase was washed with saturated aqueous NaHCO3 (3 mL), brine (5 mL) and dried over anhydrous Na2SO4, filtered and concentrated. It was purified by prep-HPLC to give (2-morpholin-4-yl-ethyl)-(3-{3-[(thiophen-2-ylmethyl)-amino]-phenyl}-1H-pyrazolo[3,4-d]pyrimidin-6-yl)-amine as yellow solid. (Yield 20 mg, 11.7%).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc (10 mL)
  3. washThe organic phase was washed with saturated aqueous NaHCO3 (3 mL), brine (5 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customIt was purified by prep-HPLC