反应详情

A mixture of compound (2) (2.83 g, 15.71 mmol), thionyl chloride (50 ml) and DMF (3 drops) was heated at reflux for 2 hours. After cooling to room temperature, excess thionyl chloride was removed under reduced pressure (rotary evaporator). The dark oil which was obtained was dissolved in carbon tetrachloride (30 ml), treated with pyridine (1 ml, 12.43 mmol) and methanol (20 ml) and stirred at ambient temperature for 2 hours. The solvents were evaporated and the residue purified by flash chromatography: silica, hexane/EtOAc (9:1).

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. customexcess thionyl chloride was removed under reduced pressure (rotary evaporator)
4. customThe dark oil which was obtained
5. customThe solvents were evaporated
6. customthe residue purified by flash chromatography