HRID1421729

反应详情

EQUATION

反应方程式

HRID 1421729 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 ester from step 2 (1.41 g, 5.317 mmol), in CH2Cl2 and methanol (1:1 50 ml) at 0° C. was treated with sodium borohydride (2.01 g, 53.17 mmol) and the reaction was stirred at room temperature for 18 hrs. The solvent was evaporated in vacuo and the residue was dissolved in EtOAc and sat. NaHCO3. The aqueous layer was extracted with EtOAc and the combined extracts were dried (MgSO4) and evaporated in vacuo. The residue was chromatographed (silica gel, MeOH: CH2Cl2 2:98 to 5:95 gradient elution) to afford the title compound.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. dissolutionthe residue was dissolved in EtOAc
  3. extractionThe aqueous layer was extracted with EtOAc
  4. dry with materialthe combined extracts were dried (MgSO4)
  5. customevaporated in vacuo
  6. customThe residue was chromatographed
  7. wash(silica gel, MeOH: CH2Cl2 2:98 to 5:95 gradient elution)