反应详情

0.215 g of 4-hydroxy-7-iodo-1-oxo-1,2-dihydro-isoquinoline-3-carboxylic acid butyl ester were added to 5 ml of POCl3 at room temperature. The mixture was refluxed for 3 h and POCl3 was removed under vacuum. The residue was dissolved in ethyl acetate and the solution was washed with satd. aqueous sodium bicarbonate, dried (MgSO4), filtered, and concentrated to give 0.205 g of a while solid: Proton NMR (200 MHz, chloroform-d) δ 11.91 (s, 1H), 8.67 (m, 1H), 8.10 (m, 2H), 4.49 (t, J=7 Hz, 2H), 1.95-1.75 (m, 2H), 1.60-1.39 (m, 2H), 1.00 (t, J=7 Hz, 3H).

1. temperatureThe mixture was refluxed for 3 h
2. customPOCl3 was removed under vacuum
3. dissolutionThe residue was dissolved in ethyl acetate
4. washthe solution was washed with satd
5. dry with materialaqueous sodium bicarbonate, dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customto give 0.205 g of a while solid