反应详情

温度

0 °C

To a mixture of 7-cyclohexylsulfanyl-1,4-dihydroxy-isoquinoline-3-carboxylic acid butyl ester (2.95 g, 7.87 mmol) in toluene (40 mL) was added POBr3 (3.38 g, 11.8 mmol) was refluxed for 3 h. Reaction mixture was cooled to 0° C. and quenched with saturated NaHCO3 aqueous solution (100 mL). It was stirred for 15 min., and then was extracted with EtOAc. Organic layer was washed with brine, dried over MgSO4, filtered and concentrated to provide the title compound 2.55 g (5.82 mmol), which was used directly to the next reaction without further purification. 1H NMR (200 MHz) CDCl3, δ in ppm: 11.85 (s, 1H), 8.23 (d, J=8.8 Hz, 1H), 8.05 (s, 1H), 7.65 (d, J=8.5 Hz, 1H), 4.47 (t, J=7.0 Hz, 2H), 3.46 (br S, 1H), 2.10 (br m, 2H), 1.85-1.42 (m, 12H), 0.99 (t, J=7.1 Hz, 3H).

1. temperaturewas refluxed for 3 h
2. customReaction mixture
3. customquenched with saturated NaHCO3 aqueous solution (100 mL)
4. extractionwas extracted with EtOAc
5. washOrganic layer was washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated