HRID1613039

反应详情

EQUATION

反应方程式

HRID 1613039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 9.0 g (0.033 mol) of 1-(6-bromohexyl)-2,3-dihydroxybenzene in 200 mL of anhydrous tetrahydrofuran and 13.7 mL (0.099 mol) of triethylamine stirred in an ice bath was added 10.9 mL (0.082 mol) of 4-methylbenzoyl chloride dropwise over 30 minutes. After 30 minutes, the bath was removed and stirring was continued at room temperature for 2.5 hours. The reaction mixture was concentrated under reduced pressure, the residue was treated with sodium bicarbonate and the product was extracted with ether. The dried extract was concentrated to an oil which was purified by HPLC using 10% ethyl acetate-hexane to give 15.2 g (90% yield) of 1-(6-bromohexyl)-2,3-bis[(4-methylbenzoyl)oxy]benzene as an oil.

WORKUP

后处理

  1. customthe bath was removed
  2. waitwas continued at room temperature for 2.5 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionthe residue was treated with sodium bicarbonate
  5. extractionthe product was extracted with ether
  6. extractionThe dried extract
  7. concentrationwas concentrated to an oil which
  8. customwas purified by HPLC