反应详情

A mixture of 1-hydroxy-4-phenyl-isoquinoline-3-carboxylic acid ethyl ester (1.17 g, 4 mmol; can be obtained according to A. Marsili et al., Ann. Chim. (Rome), 1962, 52, 112-120), and concentrated POCl3 (10 ml) was refluxed with stirring for 1 h. Then the mixture was concentrated in vacuo. The residue was dissolved in EtOAc (50 ml), concentrated aqueous NaHCO3 solution (40 ml) was added and the mixture was stirred vigorously for 1 h. Subsequently, the organic phase was separated, dried over MgSO4 and concentrated in vacuo to give the title compound as a yellowish solid (1.20 g); MS-(+)-ion: M+1=312.0.

1. customcan be obtained
2. concentrationThen the mixture was concentrated in vacuo
3. dissolutionThe residue was dissolved in EtOAc (50 ml)
4. additionconcentrated aqueous NaHCO3 solution (40 ml) was added
5. stirringthe mixture was stirred vigorously for 1 h
6. customSubsequently, the organic phase was separated
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo