反应详情

温度

120 °C

To a solution of 5-chloro-4-iodo-pyridine-2-carboxylic acid (CAN 120643-06-3, 360 mg, 1.27 mmol) in DMF (10 mL) was added with stirring Oxetan-3-ol (CAN 7748-36-9, 104 mg, 1.4 mmol) and sodium hydride 60% (107 mg, 2.67 mmol). The resulting mixture was stirred at room temperature for 30 min and at 120° C. for 25 h, cooled and the reaction mixture was concentrated in vacuo. The residue was suspended with ethylacetate, transferred into a separatory funnel and extracted with 4.0 mL of 0.5M aqueous solution hydrochloric acid. The organic phase was collected and the aqueous phase was back-extracted with ethylacetate. The organic phases were combined, dried over sodium sulfate and evaporated down to dryness to give the title compound (323 mg, 111%) as a solid which was used crude without any further purification. MS (ESI, m/z): 228.4 (M−H+)

1. temperaturecooled
2. concentrationthe reaction mixture was concentrated in vacuo
3. customtransferred into a separatory funnel
4. extractionextracted with 4.0 mL of 0.5M aqueous solution hydrochloric acid
5. customThe organic phase was collected
6. extractionthe aqueous phase was back-extracted with ethylacetate
7. dry with materialdried over sodium sulfate
8. customevaporated down to dryness