反应详情

温度

80 °C

A stirred mixture of the product from Step 1 (1.05 g, 0.00628 mol), stannous chloride dihydrate (7.09 g, 0.03141 mol) and absolute EtOH (13.9 ml), under nitrogen, was warmed to 80° C. during 30 minutes and kept at that temperature for an additional 30 minutes. The mixture was cooled and kept at ambient temperature for 1 hour. It was then poured onto ice (200 ml), treated slowly with solid NaHCO3 (2.88 g) and adjusted to pH 8 with saturated NaHCO3. This mixture was extracted with EtOAc; the extract was washed with water, dried (Na2SO4) and concentrated to give the titled product (0.738 g), a dark oil.

1. temperatureThe mixture was cooled
2. waitkept at ambient temperature for 1 hour
3. additionIt was then poured onto ice (200 ml)
4. extractionThis mixture was extracted with EtOAc
5. washthe extract was washed with water
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated