HRID543339

反应详情

EQUATION

反应方程式

HRID 543339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4-(1-methylpropoxy)phenol (0.84 g, 5.06 mmol) and potassium carbonate (0.66 g, 0.48 mmol) in 10 ml of dimethylformamide (DMF) at 5° is added ethyl 4-bromo-3-methyl-2-butenoate (1.0 g, 0.48 mmol). The mixture is allowed to warm to RT and is stirred at RT for 20 hours. The reaction mixture is poured into water and extracted with ether. The organic layer is washed with 10% sodium hydroxide to remove any starting phenol, dried and the solvent removed. The product is purified by preparative thin layer chromatography (prep. TLC). The second main band is collected to give ethyl (Z)-3-methyl-4-[4-(1-methylpropoxy)phenoxyl]-2-butenoate, MS m/e 292 (M+).

WORKUP

后处理

  1. extractionextracted with ether
  2. washThe organic layer is washed with 10% sodium hydroxide
  3. customto remove any starting phenol
  4. customdried
  5. customthe solvent removed
  6. customThe product is purified by preparative thin layer chromatography (prep. TLC)
  7. customThe second main band is collected