反应详情

温度

100 °C

To a solution in which 2-(2-(2-chloroethoxy)ethoxy)ethanol (3.48 g, 20.63 mmol) of Chemical Formula 7 was dissolved in DMF (15 mL), sodium azide (4.02 g, 61.89 mmol) was added at room temperature, and the mixture was heated to 100° C. and stirred for 12 hours. After the reaction, DMF was removed by vacuum distillation, and the residue was partitioned to distilled water (40 mL) and ethyl acetate (150 mL). The organic layer was separated, washed with saturated salted water (15 mL), dried with anhydrous sodium sulfate, and vacuum distilled, and the residue obtained was column chromatographed on silica gel (hexane/ethyl acetate (2:1)) to give 2-(2-(2-azidoethoxy)ethoxy)ethanol (3.05 g, 84%). 1H NMR (500 MHz, CDCl3) δ 3.72-3.74 (m, 2H), 3.65-3.69 (m, 6H), 3.60-3.62 (m, 2H), 3.39 (t, 2H, J=5.0 Hz).

1. customwas removed by vacuum distillation
2. customthe residue was partitioned
3. distillationto distilled water (40 mL) and ethyl acetate (150 mL)
4. customThe organic layer was separated
5. washwashed with saturated salted water (15 mL)
6. dry with materialdried with anhydrous sodium sulfate, and vacuum
7. distillationdistilled
8. customthe residue obtained
9. customchromatographed on silica gel (hexane/ethyl acetate (2:1))