反应详情

温度

120 °C

The mesylate prepared in accordance with (a) is dissolved in 100 ml of absolute dimethyl sulfoxide, and 3.2 g (35 mmoles) of the sodium salt of 1,2,4-triazole are added. The reaction mixture is stirred for 8 hours at a bath temperature of 120° C. and is then cooled to room temperature and poured into ice water, and the mixture is extracted twice with ethyl acetate. The combined extracts are washed 4 times with half-saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The crude product is purified by column chromatography (silica gel; 1:1 ethyl acetate/petroleum ether) and affords a colourless oil. n50D =1.5299. 100 MHz -1H-NMR (CDCl3): δ=7.75 and 7.65 ppm (s, 2H of triazole); 7.1-7.6 ppm (m, 2H, aromatic); 4.85 ppm (dd, 2H, CH2 -N); 4.0 ppm (m, 1H, --CH(CH3)2); 0.8-2.6 ppm (m, 14H, --CH(CH3)2, --CH2 --CH2 --CH3);

1. temperatureis then cooled to room temperature
2. extractionthe mixture is extracted twice with ethyl acetate
3. washThe combined extracts are washed 4 times with half-saturated sodium chloride solution
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product is purified by column chromatography (silica gel; 1:1 ethyl acetate/petroleum ether)
8. customaffords a colourless oil