HRID2373888

反应详情

EQUATION

反应方程式

HRID 2373888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

cis-[3-(8-Chloro-1-phenyl-imidazo[1,5-a]pyrazin-3-yl)-cyclobutyl]-dimethyl-amine: An DCE solution of 3-{1-[3-(benzyloxy)phenyl]-8-chloroimidazo[1,5-a]pyrazin-3-yl}cyclobutanone was charged with dimethylamine (0.37 mmol, 0.19 mL) and then catalytic amount of AcOH (7 μL). The mixture was stirred at rt for 30 min before resin-bound triacetoxyborohydride (0.5 mmol, 240 mg) was added. Reaction mixture was stirred at rt for 16 h before the solution was filtered through a Buchner funnel to remove the resin. The filtrate was concentrated and the obtained oil was dissolved in DCM (15 mL), washed with saturated NaHCO3 solution (2×15 mL) and brine (2×15 mL). The solvent was dried over sodium sulfate and concentrated under reduced pressure. The title compound was obtained as a yellow greasy oil; MS (ES+): m/z 433 (100) [MH+].

WORKUP

后处理

  1. additionwas added
  2. customReaction mixture
  3. filtrationwas filtered through a Buchner funnel
  4. customto remove the resin
  5. concentrationThe filtrate was concentrated
  6. dissolutionthe obtained oil was dissolved in DCM (15 mL)
  7. washwashed with saturated NaHCO3 solution (2×15 mL) and brine (2×15 mL)
  8. dry with materialThe solvent was dried over sodium sulfate
  9. concentrationconcentrated under reduced pressure