HRID539027

反应详情

EQUATION

反应方程式

HRID 539027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (S)—N2-(3-bromopyrazolo[1,5-a]pyrimidin-5-yl)-3-methylbutane-1,2-diamine (0.75 g, 2.52 mmol) in DMF was added N-ethyl-N-isopropylpropan-2-amine (1.38 ml, 7.55 mmol) and di(1H-imidazol-1-yl)methanone (0.816 g, 5.03 mmol) and the reaction stirred overnight at ambient temperature. The reaction was poured into water and extracted into EtOAc. The combined organic layers were washed with brine, dried over magnesium sulfate and concentrated in vacuo. The crude material was purified by chromatography, eluting with 2% MeOH/dichloromethane, to yield (S)-1-(3-bromopyrazolo[1,5-a]pyrimidin-5-yl)-5-isopropylimidazolidin-2-one (0.48 g, 58%).

WORKUP

后处理

  1. extractionextracted into EtOAc
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude material was purified by chromatography
  6. washeluting with 2% MeOH/dichloromethane