反应详情

To a solution of 4-amino-4-carboxy-tetrahydropyrane hydrochloride (2 g) in methanol was added dropwise a solution of 2M trimethylsilyldiazomethane-diethylether (33 mL) under ice-cooling, and the mixture was stirred at room temperature for 4 days. The reaction mixture was concentrated in vacuo, and the resultant crude product was dissolved in hexane-diethylether (1 mL/1 mL), and thereto was added an aqueous 4N hydrochloric acid. The precipitates were collected by filtration to give 4-amino-4-methoxycarbonyl-tetrahydropyrane (2.13 g, yield: 99%) as white crystals.

1. temperaturecooling
2. concentrationThe reaction mixture was concentrated in vacuo
3. dissolutionthe resultant crude product was dissolved in hexane-diethylether (1 mL/1 mL)
4. additionwas added an aqueous 4N hydrochloric acid
5. filtrationThe precipitates were collected by filtration