反应详情

As general method using H2NSO2Cl (4.63 mL, 1.39 mmol), DMA (1.5 mL) and 19 (0.077 g, 0.279 mmol). The reaction mixture was poured into EtOAc (30 mL). The organic layer separated was washed with distilled H2O (30 mL×4), brine (30 mL), dried (MgSO4) and evaporated in vacuo to give white residues. Column chromatography (CH2Cl2/acetone 80:20) eluted 15 as a white solid (0.074 g, 75%), mp 159-162° C.; 1H NMR δH (270 MHz, DMSO-d6) 5.60 (s, 2H), 7.41-7.46 (m, 314), 7.51 (s, 1H), 7.67 (d, J=8.2, 2H), 7.98 (d, J=7.9, 1H), 8.03 (s, 1H), 8.17 (br s, 214) and 8.73 (s, 1H);

1. customThe organic layer separated
2. washwas washed with distilled H2O (30 mL×4), brine (30 mL)
3. dry with materialdried (MgSO4)
4. customevaporated in vacuo
5. customto give white residues
6. washColumn chromatography (CH2Cl2/acetone 80:20) eluted 15 as a white solid (0.074 g, 75%), mp 159-162° C.