HRID1769384

反应详情

EQUATION

反应方程式

HRID 1769384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with EtOAc (3×30 mL)
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe resulting residue was purified by flash chromatography (eluant:EtOAc-hexane-HOAc (250:750:1))