反应详情

Commercially available furan-2,4(3H,5H)-dione (0.433 g, 4.33 mmol) and tert-butyl 2,8-diazaspiro[4.5]decane-8-carboxylate (commercially available from multiple vendors, acetic acid salt, 0.65 g, 2.2 mmol) in 20 mL i-PrOH was heated in a sealed tube at 110° C. overnight. The solid was filtered off and the filtrate was concentrated under vacuum. The residue was dissolved in 30 mL DCM and 5 mL TFA and stirred at rt for 1 h. The mixture was concentrated, and the residue was purified by preparative TLC (10% 2N NH3 in methanol-DCM). LCMS: [(M+1)]+=223

1. filtrationThe solid was filtered off
2. concentrationthe filtrate was concentrated under vacuum
3. dissolutionThe residue was dissolved in 30 mL DCM
4. concentrationThe mixture was concentrated
5. customthe residue was purified by preparative TLC (10% 2N NH3 in methanol-DCM)