反应详情

温度

60 °C

Hydroxylamine hydrochloride (24.51 g, 353 mmol) was added to a mixture of 1,1-dimethylethyl 3-(5-cyano-1-isoquinolinyl)propanoate (D35; 24.9 g, 88 mmol) and sodium bicarbonate (44.5 g, 529 mmol) in ethanol (200 ml) and the mixture heated at 60° C. for 5 h. The cooled mixture was filtered and the filtrate concentrated in vacuo. The residue was partitioned between water (100 ml) and ethyl acetate (3×100 ml) and the combined organic extracts washed with brine (100 ml) and dried (MgSO4). The solvent was evaporated to give a pale yellow solid which was triturated under ether (100 ml) and filtered to give the title compound as a colourless solid (19.91 g)

1. filtrationThe cooled mixture was filtered
2. concentrationthe filtrate concentrated in vacuo
3. customThe residue was partitioned between water (100 ml) and ethyl acetate (3×100 ml)
4. washthe combined organic extracts washed with brine (100 ml)
5. dry with materialdried (MgSO4)
6. customThe solvent was evaporated
7. customto give a pale yellow solid which
8. customwas triturated under ether (100 ml)
9. filtrationfiltered