HRID1394226
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 sodium phenoxide (prepared from phenol and NaH) (6 mmol) in THF (3 mL) was added to a solution of the product from Step 1 (600 mg, 3.0 mmol) in THF (2 mL) and the resulting solution was heated to reflux overnight. The solution was cooled, poured into H2O and extracted with EtOAc. The organic layers were washed with H2O and brine, dried, filtered and concentrated to give a residue which was purified by column chromatography (5-80% EtOAc in hex) to give the title compound which was used directly in the next step. MS (ES+) m/e 260. [M+H]+.
WORKUP
后处理
- temperaturethe resulting solution was heated
- temperatureto reflux overnight
- temperatureThe solution was cooled
- extractionextracted with EtOAc
- washThe organic layers were washed with H2O and brine
- customdried
- filtrationfiltered
- concentrationconcentrated
- customto give a residue which
- customwas purified by column chromatography (5-80% EtOAc in hex)