tert-butyl N-[[1-(hydroxymethyl)cyclobutyl]methyl]carbamate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of tert-butyl {[1-(hydroxymethyl)cyclobutyl]methyl}carbamate (12 g, 55.76 mmol), diethyl 1H-indole-2,6-dicarboxylate (14.56 g, 55.76 mmol) and triphenylphosphine (29.2 g, 111.5 mmol.) in THF (110 mL) is added diisopropyl azodicarboxylate (22.41 mL, 111.5 mmol) at room temperature and the reaction mixture is stirred for 60 h. The solvent is evaporated and the residue is purified by flash column chromatography using 12% EtOAc in petroleum ether to afford diethyl 1-[(1-{[(tert-butoxycarbonyl)amino]methyl}cyclobutyl)methyl]-1H-indole-2,6-dicarboxylate contaminated with un-reacted diethyl 1H-indole-2,6-dicarboxylate. The mixture is used in the next step without further purification. The solvent is evaporated the residue is purified by flash column chromatography