反应详情

温度

80 °C

A stirred mixture of the product from Step 1 (7.70 g, 0.0461 mol) and stannous chloride dihydrate (56.4 g, 0.250 mol) in absolute EtOH (100 ml) was warmed to 80° C. during 15 minutes and kept at that temperature for 35 minutes. The resulting mixture was kept at ambient temperature for 1 hour, poured onto ice (400 ml) and mixed with NaHCO3 (15 g). It was adjusted to a pH of 8-9 with saturated aqueous NaHCO3 and extracted with EtOAc; the extract was washed with water and brine dried (MgSO4) and concentrated to give 5.98 g of crude product. Pan of this was purified by silica gel chromatography, with 5% MeOH--0.25% NH4OH--CHCl3 to give the titled product.

1. waitThe resulting mixture was kept at ambient temperature for 1 hour
2. additionpoured onto ice (400 ml)
3. extractionextracted with EtOAc
4. washthe extract was washed with water and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customto give 5.98 g of crude product
8. customPan of this was purified by silica gel chromatography, with 5% MeOH--0.25% NH4OH--CHCl3