反应详情

温度

65 °C

To a solution of the crude ester from Step 4 above in 25 mL of a 3:1:1 mixture of THF:MeOH:water, was added 5.1 mL (10.3 mmol) of a 2 N solution of LiOH. The resulting solution was stirred at 65° C. for 1.5 h, cooled down to room temperature followed by the addition of 10 mL of a 1.0 N HCl solution. The resulting mixture was rotovaped down to evaporate MeOH and the aqueous residue was diluted with ethyl acetate. The organic layer was washed with water and brine, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (50% Ethyl acetate/hexane) to afford the desired pyridine as an oil (380 mg, 68% from Step 2).

1. temperaturecooled down to room temperature
2. customto evaporate MeOH
3. additionthe aqueous residue was diluted with ethyl acetate
4. washThe organic layer was washed with water and brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by flash chromatography on silica gel (50% Ethyl acetate/hexane)
8. customto afford the desired pyridine as an oil (380 mg, 68% from Step 2)