反应详情

250 mmol of n-butyllithium (1.6M solution in n-hexane) are added dropwise at 0° C. with exclusion of moisture and under a protective-gas atmosphere to a solution of 250 mmol of 5bromo-2-hexyloxypyridine in 500 ml of abs. diethyl ether. The mixture is stirred at this temperature for a further 1 hour, and 275 mmol of trimethyl borate are subsequently added slowly. After the mixture has been stirred at 0° C. for a further hour, a solution of 175 ml of water and 25 ml of 37 percent hydrochloric acid is added dropwise. The mixture is stirred at room temperature for 1 hour, the phases are then separated, the aqueous phase is extracted a number of times with dichloromethane, and the combined organic extracts are dried using magnesium sulfate. The solvents are removed in vacuo. After drying in a high vacuum, the red-brown, high-viscosity crude product is reacted further without additional purification.

1. stirringAfter the mixture has been stirred at 0° C. for a further hour
2. stirringThe mixture is stirred at room temperature for 1 hour
3. customthe phases are then separated
4. extractionthe aqueous phase is extracted a number of times with dichloromethane
5. customthe combined organic extracts are dried
6. customThe solvents are removed in vacuo
7. customAfter drying in a high vacuum
8. customthe red-brown, high-viscosity crude product is reacted further without additional purification