HRID1692952

反应详情

EQUATION

反应方程式

HRID 1692952 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(Bromomethyl)-1-[4-(7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]cyclobutylacetonitrile (0.65 g, 0.0013 mol) was reacted with sodium tetrahydroborate (0.096 g, 0.0026 mol) in DMF (5.2 mL) (˜0.5 M) at rt under nitrogen for 3h. The reaction was quenched with water and extracted with dichloromethane. The organic layers were washed with water, brine, dried over MgSO4 and concentrated to give a yellow oil, the desired product as cis- and trans-isomer mixtures. LCMS calculated for C22H31N6OSi(M+H)+: 423.2; Found: 423.4.

WORKUP

后处理

  1. customThe reaction was quenched with water
  2. extractionextracted with dichloromethane
  3. washThe organic layers were washed with water, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customto give a yellow oil