HRID2047168

反应详情

EQUATION

反应方程式

HRID 2047168 的结构方程式

PROCEDURE

实验过程

To a solution of compound, 5-(tetrahydro-2H-thiopyran-4-yl)-N,N-bis((2-(trimethylsilyl)ethoxy)methyl)pyrazolo[1,5-a]pyrimidin-7-amine (18.7 mmol, 9.23 g) DCM (100 mL) was added mCPBA and stirred at rt for 1 h. The reaction was quenched with Na2S2O3 (aq.) and diluted with DCM (100 mL). The separated organic layer was washed with NaHCO3 (2*) and brine, dried over Na2SO4, and concentrated to afford crude compound, 5-(tetrahydro-2H-thiopyran-4-yl-1′,1′-dioxide)-)-N,N-bis((2-(trimethylsilyl)ethoxy)methyl)pyrazolo[1,5-a]pyrimidin-7-amine as a purple oil, which was used without further purification. HPLC-MS TR=2.72 min (UV 254 nm, 5 min method); mass calculated for formula C23H42N4O4SSi2 526.2, observed LCMS m/z 527.2 (M+H).

WORKUP

后处理

  1. customThe reaction was quenched with Na2S2O3 (aq.)
  2. additiondiluted with DCM (100 mL)
  3. washThe separated organic layer was washed with NaHCO3 (2*) and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated