HRID1617163

反应详情

EQUATION

反应方程式

HRID 1617163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from step (iv) (1.52 g) in THF (30 mL) was added portionwise to a stirred solution of lithium aluminium hydride (1M in THF; 8.43 mL) in THF (30 mL) at 0° C. under nitrogen. The resulting mixture was stirred at rt for 2 h. EtOAc (10 mL) was added cautiously to the reaction mixture and the mixture added portionwise to 2M NaOH (100 mL). The mixture was stirred for 30 min and the aqueous solution was extracted with EtOAc. The combined organic phase was dried, filtered and evaporated. The crude product was purified by chromatography elutinhg with 2 to 5% MeOH in acetonitrile to give the subtitle compound as a yellow oil 0.85 g.

WORKUP

后处理

  1. stirringThe mixture was stirred for 30 min
  2. extractionthe aqueous solution was extracted with EtOAc
  3. customThe combined organic phase was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude product was purified by chromatography elutinhg with 2 to 5% MeOH in acetonitrile