HRID247611

反应详情

EQUATION

反应方程式

HRID 247611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. dissolutionthe residue is dissolved in 800 ml of toluene
  3. extractionThe toluene solution is extracted sequentially with 1M sodium hydroxide (2×100 ml) and water (6×200 ml)
  4. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  5. customThe solvent is removed in vacuo
  6. customthe residue purified by flash chromatography (8:2 heptane: ethyl acetate eluent)
  7. customfollowed by recrystallization from petroleum ether