HRID1267107

反应详情

EQUATION

反应方程式

HRID 1267107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of magnesium (0.69 g) in Et2O (5 mL) containing a trace of iodine was added dropwise a solution of 1-bromo4-isopropyl-benzene (5.97 g) in Et2O (50 mL). Following the addition, the mixture was heated under reflux for 1 hour. The resulting grignard solution was then carrefully added to a solution of 2-(2,4-dimethoxy-phenyl)-4,4-dimethyl-4,5-dihydro-oxazole (3.52 g) in THF (60 mL) and the mixture was stirred at room temperature for 16 hours. The reaction mixture was then poured into saturated aqueous solution of NH4Cl and the mixture was extracted with Et2O, dried over Na2SO4, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography eluting with CH2Cl2/AcOEt (85/15) to give the title compound (3.5 g) as a pale yellow oil.

WORKUP

后处理

  1. additionthe addition
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1 hour
  4. extractionthe mixture was extracted with Et2O
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe residue was purified by flash chromatography
  9. washeluting with CH2Cl2/AcOEt (85/15)