HRID574060
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 a solution of powdered KOH (45 mg, 0.8 mM) in anhydrous DMSO (2.5 mL) at room temperature was added 3-{[4-(4,4-Dimethyl-4,5-dihydro-oxazol-2-yl)-phenyl]-hydroxy-phenyl-methyl}-phenol (2, 150 mg, 0.4 mM) and (3-Bromo-propyl)-carbamic acid tert-butyl ester (96 mg, 0.4 mM). The reaction mixture was stirred at room temperature for 3 h. Then the reaction mixture was extracted with ethyl acetate (3×25 mL) and the combined extract was dried over anhydrous Mg2SO4. The residue obtained on evaporation of the solvent was purified by silica gel chromatography using hexane/EtOAc (1:1) as an eluent. Evaporation of the solvent gave 3. Yield: >220 mg (quantitative yield). Mass: 531 (MH+).
WORKUP
后处理
- extractionThen the reaction mixture was extracted with ethyl acetate (3×25 mL)
- extractionthe combined extract
- dry with materialwas dried over anhydrous Mg2SO4
- customThe residue obtained on evaporation of the solvent
- customwas purified by silica gel chromatography
- customEvaporation of the solvent
- customgave 3