反应详情

2,6-Dichloroquinoline (15.2 moles, 3.0 g), 4-aminothiophenol (15.2 moles, 1.9 g), and DMAP (15.2 moles, 1.85 g) were stirred at room temperature for 3 days. The solvent was removed, diluted with ethyl acetate, washed with water, dried over sodium sulfate and concentrated. The product was purified by HPLC over silica gel eluted with 25% ethyl acetate in hexane to yield 2-(4-aminophenylthio)-6-chloroquinoline 830 mg, 19%. Mass spec (FD) 286. Calculated for C15H11ClN2S: C, 62.82 H, 3.87; N, 9.77. Found: C, 63.09; H, 3.94; N, 9.61.

1. customThe solvent was removed
2. additiondiluted with ethyl acetate
3. washwashed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe product was purified by HPLC over silica gel
7. washeluted with 25% ethyl acetate in hexane