反应详情

To a stirred solution of methyl 5-methyl-6-(2,2,2-trifluoroethoxy)nicotinate (0.80 g, 3.21 mmol, Step-1) in THF (10 mL) is added slowly lithium aluminum hydride (0.11 g, 3.21 mmol) at 0° C. The resulting mixture is stirred at rt for 1 hour. The reaction mixture is carefully quenched with 25% aqueous ammonia solution at 0° C. Then the mixture is diluted with DCM (50 mL) and celite is added to the mixture. After stirring at rt for 1 hour, the mixture is filtrated through a pad of Celite, and the filtrate is concentrated in vacuo to give 0.70 g (99% yield) of the title compound as colorless oil. This material is used for the next reaction (Step-3) 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 DCM (50 mL) and celite
3. additionis added to the mixture
4. stirringAfter stirring at rt for 1 hour
5. filtrationthe mixture is filtrated through a pad of Celite
6. concentrationthe filtrate is concentrated in vacuo