反应详情

To a stirred suspension of 2-aminomethyl-3-chloropyrazine hydrochloride (3.89 mmol, 0.70 g) in dichloromethane (25 mL) at room temperature was subsequently added triethylamine (7.78 mmol, 1.08 mL), O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluroniumhexafluorophosphate (4.67 mmol, 1.77 g) and finally 4-oxocyclohexanecarboxylate (3.89 mmol, 553 mg). After stirring for 16 hours, the suspension filtered over decalite. The decalite was washed with dichloromethane. The filtrate was washed with water, dried (sodium sulfate) and concentrated in vacuo. The resulting crude product was purified by column chromatography on silica gel (ethyl acetate). The product was dissolved in dichloromethane, washed with water and concentrated in vacuo to afford 1.09 g of the title compound.

1. filtrationthe suspension filtered over decalite
2. washThe decalite was washed with dichloromethane
3. washThe filtrate was washed with water
4. dry with materialdried (sodium sulfate)
5. concentrationconcentrated in vacuo
6. customThe resulting crude product was purified by column chromatography on silica gel (ethyl acetate)
7. dissolutionThe product was dissolved in dichloromethane
8. washwashed with water
9. concentrationconcentrated in vacuo