反应详情

温度

37 °C

In a brown flask, L-glucosamine hydrochloride (40.0 mg) and NaHCO3 (26.0 mg) were placed and dissolved in water (800 μl). A solution in which 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) (92.0 mg) was dissolved in methanol (4.0 ml) was added thereto, and under an argon atmosphere, the resulting mixture was stirred for 2 hours at a bath temperature of 37° C. Thereafter, the mixture was stirred at room temperature for an additional 40 minutes. Methanol was removed by concentration under reduced pressure, and the resulting precipitates (unnecessary substances derived from NBD-F) were removed by filtration. The precipitates were washed with water, and the filtrate and the washing solution were combined, followed by purification by HPLC. A target fraction was collected and lyophilized, whereby a target product was obtained (yield: 48.7 mg, yield ratio: 76%).

1. additionwas added
2. stirringThereafter, the mixture was stirred at room temperature for an additional 40 minutes
3. customMethanol was removed by concentration under reduced pressure
4. customthe resulting precipitates (unnecessary substances derived from NBD-F)
5. customwere removed by filtration
6. washThe precipitates were washed with water
7. customfollowed by purification by HPLC
8. customA target fraction was collected
9. customwhereby a target product was obtained
10. custom(yield: 48.7 mg, yield ratio: 76%)