反应详情

温度

100 °C

Aq. 5M KOH (0.5 mL) was added to a stirred solution of the product from step (v) (70 mg) in butan-1-ol (1 mL) and heated to 100° C. for 15 h. The mixture was allowed to cool, diluted with water (2 mL) and then adjusted to ˜pH 7 with conc. HCl. The organic phase was separated and the aqueous was extracted with butan-1-ol (5 mL). The combined organic extracts were evaporated, the residue was dissolved in MeOH and conc. HCl (0.3 mL) was added and the mixture heated to 70° C. for 1 h. After cooling the reaction was poured into sat. NaHCO3 (10 mL) and extracted with EtOAc, dried and the solvent removed. The crude product was purified by RPHPLC to afford the title compound as a colourless gum, 22 mg.

1. temperatureto cool
2. customThe organic phase was separated
3. extractionthe aqueous was extracted with butan-1-ol (5 mL)
4. customThe combined organic extracts were evaporated
5. dissolutionthe residue was dissolved in MeOH
6. additionconc. HCl (0.3 mL) was added
7. temperaturethe mixture heated to 70° C. for 1 h
8. temperatureAfter cooling the reaction
9. additionwas poured into sat. NaHCO3 (10 mL)
10. extractionextracted with EtOAc
11. customdried
12. customthe solvent removed
13. customThe crude product was purified by RPHPLC