反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added
- customReaction mixture
- filtrationwas filtered through a Buchner funnel
- customto remove the resin
- concentrationThe filtrate was concentrated
- dissolutionthe obtained oil was dissolved in DCM (15 mL)
- washwashed with saturated NaHCO3 solution (2×15 mL) and brine (2×15 mL)
- dry with materialThe solvent was dried over sodium sulfate
- concentrationconcentrated under reduced pressure