反应详情

4.71 g of 2,4-dimethylthiazole-5-carboxylic acid was suspended in 70 ml of tetrahydrofuran, and 6.67 g of triethylamine was added. The mixture was stirred. While it was cooled to -10° to -5° C., 4.10 g of n-butyl chloroformate was added, and the mixture was stirred at this temperature for 30 minutes, and then 4.03 g of alpha-(2-furyl)-alpha-aminoacetonitrile hydrochloride was added. The mixture was stirred at room temperature for 5 hours, and then left to stand overnight. The precipitate was separated by filtration and distilled under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography. Elution with hexane/ethyl acetate gave 4.20 g (yield 53.6%) of the desired N-(alpha-cyanofurfuryl)-2,4-dimethylthiazole-5-carboxylic acid amide.

1. temperatureWhile it was cooled to -10° to -5° C.
2. stirringthe mixture was stirred at this temperature for 30 minutes
3. stirringThe mixture was stirred at room temperature for 5 hours
4. waitleft
5. customThe precipitate was separated by filtration
6. distillationdistilled under reduced pressure
7. customto remove the solvent
8. customThe residue was purified by silica gel column chromatography
9. washElution with hexane/ethyl acetate