HRID399339

反应详情

EQUATION

反应方程式

HRID 399339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 g (8.28 mmol) of epoxide 2j in solution in 5 cm3 of anhydrous DMF were heated to reflux for 5 h. The solution was acidified (pH<1) with 3N HCl, extracted with ether and concentrated, and a 3N sodium hydroxide solution was added to the ether phase (while the mixture was kept stirred for 5 to 10 min), the ether phase was removed and the material washed once with ether. The aqueous phase was acidified using a solution with 3N HCl (pH=1) and extracted with ether (4×30 cm3), dried over MgSO4, filtered and evaporated down. 1.24 g of phenol 4g were obtained as a liquid whose macrobore GC purity was higher than 97%. The yield of phenol 4g was 89%.

WORKUP

后处理

  1. temperatureto reflux for 5 h
  2. extractionextracted with ether
  3. concentrationconcentrated
  4. additiona 3N sodium hydroxide solution was added to the ether phase (while the mixture
  5. customwas removed
  6. washthe material washed once with ether
  7. extractionextracted with ether (4×30 cm3)
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated down