HRID2261246
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 mixture of methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester (Intermediate 6) (1.37 g, 5.18 mmol) and lithium bromide (1.80 g, 20.7 mmol) in acetone (15 mL) was heated at reflux overnight. The reaction mixture was concentrated to dryness and the residue partitioned between DCM and water. The organic layer was dried (MgSO4), and concentrated, and purified by column chromatography over silica using DCM/cyclohexane (1:3) as eluent to afford the product as a colourless oil.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux overnight
- concentrationThe reaction mixture was concentrated to dryness
- customthe residue partitioned between DCM and water
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated
- custompurified by column chromatography over silica