HRID1912897
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
To the 500 mL round bottom flask with the product from Example 10A was added 100 mL ethanol. The mixture was cooled in an ice bath (NaCl was added to the bath to keep the temperature below 0° C.) and sodium borohydride was added. The mixture was stirred for 30 minutes. 160 mL 0.5 N HCl solution was added carefully and ethyl acetate was used to extract the mixture twice. Brine was added to help the layers to separate. The combined organic layers were washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo. The crude title compound was used directly in the following steps without further purification. MS (ESI) m/z 135.1 (M−H)−.
WORKUP
后处理
- additionwas added to the bath
- customthe temperature below 0° C.
- additionwas added
- extractionto extract the mixture twice
- additionBrine was added
- customto separate
- washThe combined organic layers were washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude title compound was used directly in the following steps without further purification