反应详情

温度

-20 °C

n-Butyl-isobutyramide (0.99 g, 0.0069 m) in dry THF (10 ml) was cooled to -20° C. under nitrogen during the dropwise addition of a 1.445 M solution of n-butyl lithium (4.8 ml, 0.0069 m). The mixture was stirred for 20 minutes at -20° C. and then 4-methyl-2-methylsulphinyloxazole (1.0 g, 0.0068 m) in dry THF (10 ml) was added rapidly and the mixture allowed to warm to 0° C. It was stirred at this temperature for 11/2 hours then allowed to warm to room temperature and stirred for a further 1/2 hour. The mixture was hydrolysed with water and the solvent was evaporated under reduced pressure. The residue was extracted with diethyl ether and the extract was evaporated. The resulting oil was chromatographed on silica using ether/hexane. The compound was distilled in vacuo to give the title compound as a colourless oil 1.21 g, (78%), b.p. (airbath) 70° C. at 0.01 mm.

1. temperatureto warm to 0° C
2. stirringIt was stirred at this temperature for 11/2 hours
3. temperatureto warm to room temperature
4. stirringstirred for a further 1/2 hour
5. customthe solvent was evaporated under reduced pressure
6. extractionThe residue was extracted with diethyl ether
7. customthe extract was evaporated
8. customThe resulting oil was chromatographed on silica
9. distillationThe compound was distilled in vacuo