HRID1585907
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
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
- customThe solvent was evaporated in vacuo
- dissolutionthe residue was dissolved in EtOAc
- extractionThe aqueous layer was extracted with EtOAc
- dry with materialthe combined extracts were dried (MgSO4)
- customevaporated in vacuo
- customThe residue was chromatographed
- wash(silica gel, MeOH: CH2Cl2 2:98 to 5:95 gradient elution)