反应详情

To 1.21 g (4.76 mmol) iodine in 50 mL toluene is added 1.59 g (4.76 mmol) polymer bound triphenyl-phosphane. The mixture is stirred 5 min at RT and then 0.80 mL (9.92 mmol) pyridine and 1.10 g (3.97 mmol) 7-(2-hydroxy-ethyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (preparation 7c) is added. The reaction mixture is stirred 5 h at 90° C., is cooled to RT and is filtered. The filtrate is washed with saturated aqueous sodium thiosulfate-solution, brine and dried over MgSO4. After filtration and evaporation of the solvent, the residue is purified via chromatography (silica gel; PE/EtOAc=9:1).

1. stirringThe reaction mixture is stirred 5 h at 90° C.
2. temperatureis cooled to RT
3. filtrationis filtered
4. washThe filtrate is washed with saturated aqueous sodium thiosulfate-solution, brine
5. dry with materialdried over MgSO4
6. filtrationAfter filtration and evaporation of the solvent
7. customthe residue is purified via chromatography (silica gel; PE/EtOAc=9:1)