反应详情

温度

-5 °C

To 2.30 g (7.18 mmol) 6-(methoxy-methyl-carbamoyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (preparation 29a) in 50 mL THF is added under an argon atmosphere at 0° C. 7.18 mL (21.5 mmol; 3 M solution in diethylether) methylmagnesium bromide. The reaction mixture is stirred 1.5 h at −5° C. and is then transferred into a saturated aqueous ammonium chloride solution. The aqueous phase is extracted three times with tert-butylmethylether, dried over MgSO4, filtered and the solvent is evaporated. The residue is purified by silica gel column chromatography with PE/EtOAc (8:2) as eluent.

1. extractionThe aqueous phase is extracted three times with tert-butylmethylether
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customthe solvent is evaporated
5. customThe residue is purified by silica gel column chromatography with PE/EtOAc (8:2) as eluent