反应详情

Diisopropyl azodicarboxylate (0.105 mL, 0.54 mmol) is added to a solution of [2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]-3-pyridyl]methanol (0.173 g, 0.36 mmol), phthalimide (0.079 mg, 0.54 mmol) and triphenylphosphine (0.142 g, 0.54 mmol) in toluene (3 mL) at 0° C. The mixture is stirred at room temperature overnight. The solvent is removed and the residue is purified first using a 2 g SCX cartridge and after evaporation of the 2 N ammonia in methanol fraction by normal phase Isco chromatography eluting with hexane/ethanol (3%-30%) to give 0.201 g of 2-[[2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]-3-pyridyl]methyl]isoindoline-1,3-dione. MS (m/z): 610 (M+1).

1. customThe solvent is removed
2. customthe residue is purified first
3. customafter evaporation of the 2 N ammonia in methanol fraction by normal phase Isco chromatography
4. washeluting with hexane/ethanol (3%-30%)