反应详情

To 1.40 g (5.09 mmol) 6-acetyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (preparation 29b) in 20 mL THF is added a solution of 2.45 g (5.09 mmol) tetrabutylammonium-tribromide in MeOH/THF at RT. The reaction mixture is stirred 30 min at RT and the solvent is evaporated. The residue is treated with water and 1 M aqueous HCl-solution and the aqueous phase is extracted with tert-butylmethylether. The organic phase is washed with water and 1 M aqueous HCl-solution, dried over MgSO4, filtered and the solvent is evaporated. The residue is purified by silica gel column chromatography with PE/EtOAc (7:3) as eluent.

1. customthe solvent is evaporated
2. additionThe residue is treated with water and 1 M aqueous HCl-solution
3. extractionthe aqueous phase is extracted with tert-butylmethylether
4. washThe organic phase is washed with water and 1 M aqueous HCl-solution
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customthe solvent is evaporated
8. customThe residue is purified by silica gel column chromatography with PE/EtOAc (7:3) as eluent