反应详情

温度

220 °C

A mixture of 200 mg 1-chloro-2-(4-acetoxy-benzyl)-4-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranos-1-yl)-benzene, 35 mg sodium cyanide and 75 mg nickel bromide in 0.5 mL N-methyl-2-pyrrolidinone is heated in a microwave oven at 220° C. for 15 min. After cooling to room temperature, water is added and the resultant mixture is extracted with ethyl acetate. After drying over sodium sulfate and evaporation of the solvent, the residue is dissolved in 3 mL methanol. 3 mL of 4 M aqueous potassium hydroxide solution is added and the reaction solution is stirred at ambient temperature for 3 h. The solution is neutralized with 1 M hydrochloric acid and the methanol is evaporated. The residue is extracted with ethylacetate, the combined extracts are dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by HPLC on reversed phase (YMC C18; water/acetonitrile 95:5->1:99).

1. temperatureAfter cooling to room temperature
2. extractionthe resultant mixture is extracted with ethyl acetate
3. dry with materialAfter drying over sodium sulfate and evaporation of the solvent
4. dissolutionthe residue is dissolved in 3 mL methanol
5. addition3 mL of 4 M aqueous potassium hydroxide solution is added
6. customthe methanol is evaporated
7. extractionThe residue is extracted with ethylacetate
8. dry with materialthe combined extracts are dried over sodium sulfate
9. customthe solvent is removed under reduced pressure
10. customThe residue is purified by HPLC on reversed phase (YMC C18; water/acetonitrile 95:5->1:99)