反应详情

To a stirred solution of methyl 6-(2,2,2-trifluoroethoxy)picolinate (0.40 g, 1.69 mmol, Step-2) in tetrahydrofuran (17 mL) is added slowly lithium aluminum hydride (0.096 g, 2.53 mmol) at 0° C. The resulting mixture is stirred at room temperature for 1 hour. The reaction mixture is carefully quenched with 25% aqueous ammonia solution at 0° C. Then the mixture is diluted with dichloromethane (50 mL) and celite is added to the mixture. After stirring at room temperature for 1 hour, the mixture is filtrated through a pad of celite, and the filtrate is concentrated in vacuo to give 0.32 g (92% yield) of the title compound as a white solid. This material is used for the next reaction (Step-4) without further purification.

1. customThe reaction mixture is carefully quenched with 25% aqueous ammonia solution at 0° C
2. additionThen the mixture is diluted with dichloromethane (50 mL) and celite
3. additionis added to the mixture
4. stirringAfter stirring at room temperature for 1 hour
5. filtrationthe mixture is filtrated through a pad of celite
6. concentrationthe filtrate is concentrated in vacuo