反应详情

温度

90 °C

A mixture of 5-(chloromethyl)-3-methyl-2-(2,2,2-trifluoroethoxy)pyridine (0.75 g, 3.15 mmol, Step-3) and sodium azide (0.41 g, 6.29 mmol) in DMA (8 mL) is stirred at 90° C. for 2 hours. The reaction mixture is poured into water (50 mL), and extracted with n-hexane/EtOAc (1:10, 50 mL). The organic layer is washed with water (50 mL) and dried over sodium sulfate. After filtration, the organic fraction is concentrated in vacuo to give 0.77 g (>99% yield) of the title compound as colorless oil. This material is used for the next reaction (Step-5) without further purification.

1. extractionextracted with n-hexane/EtOAc (1:10, 50 mL)
2. washThe organic layer is washed with water (50 mL)
3. dry with materialdried over sodium sulfate
4. filtrationAfter filtration
5. concentrationthe organic fraction is concentrated in vacuo