HRID324296
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
3-(2-Quinolinyl-methoxy)phenol (12.5 g), potassium carbonate (10.4 g) and 1,3-dioxolan-2-one (44 g) were stirred on an oil bath at 100° C. for 2 hours. The mixture was cooled, poured into water and extracted with DCM. The organic layer was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3). The pure fractions were collected and evaporated. The residue was stirred up in DIPE. The precipitate was filtered off and dried, yielding 11.9 g (80.6%) of 2-[3-(2-quinolinyl-methoxy)phenoxy]ethanol (intermediate 5).
WORKUP
后处理
- temperatureThe mixture was cooled
- extractionextracted with DCM
- customThe organic layer was dried
- filtrationfiltered
- customevaporated
- customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3)
- customThe pure fractions were collected
- customevaporated
- filtrationThe precipitate was filtered off
- customdried