HRID247611
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
This compound is prepared by the procedure of Example 1 from 2.40 g (0.1 mol) of sodium hydride, 20.63 g (0.1 mol) of 2,6-di-tert-butylphenol, and 26.54 g (0.1 mol) of N-n-dodecylmaleimide in tert-butyl alcohol. The reaction mixture is concentrated in vacuo and the residue is dissolved in 800 ml of toluene. The toluene solution is extracted sequentially with 1M sodium hydroxide (2×100 ml) and water (6×200 ml). The organic phase is dried over anhydrous sodium sulfate. The solvent is removed in vacuo and the residue purified by flash chromatography (8:2 heptane: ethyl acetate eluent) followed by recrystallization from petroleum ether to give 8.15 g (17%) of a white solid: mp 66°-70° C.
WORKUP
后处理
- concentrationThe reaction mixture is concentrated in vacuo
- dissolutionthe residue is dissolved in 800 ml of toluene
- extractionThe toluene solution is extracted sequentially with 1M sodium hydroxide (2×100 ml) and water (6×200 ml)
- dry with materialThe organic phase is dried over anhydrous sodium sulfate
- customThe solvent is removed in vacuo
- customthe residue purified by flash chromatography (8:2 heptane: ethyl acetate eluent)
- customfollowed by recrystallization from petroleum ether