反应详情

The acid 18-5 (810 mg) was dissolved in 40 mL 1 N NaOH and 40 mL MeOH at room temperature and was treated with Raney nickel suspension (˜5 g). A second charge of Raney nickel (˜5 g) and 1 N NaOH (20 mL) was added after 3 h. After 6 h, the suspension was filtered through celite washing with water and MeOH. The volatiles were removed in vacuo and the residue then taken up 1 N HCl (˜5 mL). Saturated NaHCO3 solution was added until pH˜7-8 and the solution was extracted exhaustively with EtOAc/THF. After drying (MgSO4), the solvent was removed to give the title compound 18-6 as a solid which was used as such:

1. additionwas added after 3 h
2. filtrationthe suspension was filtered
3. washthrough celite washing with water and MeOH
4. customThe volatiles were removed in vacuo
5. additionSaturated NaHCO3 solution was added until pH˜7-8
6. extractionthe solution was extracted exhaustively with EtOAc/THF
7. dry with materialAfter drying (MgSO4)
8. customthe solvent was removed