反应详情

To a solution of 1.0 g of tert-butyl 4-hydroxy-6-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)spiro[chroman-2,4′-piperidine]-1′-carboxylate in 40 ml of THF-CH3CN (1:1) at r.t. were added 2.0 g of MS 4A, 435 mg of NMO, and 88 mg of TPAP, and the reaction mixture was stirred at r.t. overnight. The mixture was filtered through a Celite pad, washed with CHCl3 and CHCl3-MeOH (9:1), and the filtrate was concentrated in reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of hexane-AcOEt (100/0-0/100) as eluent to give the intended compound as a colorless solid.

1. filtrationThe mixture was filtered through a Celite pad
2. washwashed with CHCl3 and CHCl3-MeOH (9:1)
3. concentrationthe filtrate was concentrated in reduced pressure
4. customThe residue was purified by column chromatography on silica gel using
5. additiona mixture of hexane-AcOEt (100/0-0/100) as eluent