HRID1769384
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
The compound from Step E was hydrolysed using THF (2.5 mL), MeOH (0.6 mL) and NaOH (1N, 1.5 mL). The solution was heated at 70° C. for 2 weeks. The reaction was neutralized by addition of Na4OAc buffer (20 mL of 25% w/v) and extracted with EtOAc (3×30 mL). The organic layers were combined, dried over MgSO4, filtered and concentrated. The resulting residue was purified by flash chromatography (eluant:EtOAc-hexane-HOAc (250:750:1)) to give the title compound. Anal. C, H, N for sodium salt·11/2 H2O; Calc. C, 67.70; H, 6.43; N, 4.15 Found C, 67.67; H, 6.31; N, 4.06.
WORKUP
后处理
- extractionextracted with EtOAc (3×30 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe resulting residue was purified by flash chromatography (eluant:EtOAc-hexane-HOAc (250:750:1))