HRID981437

反应详情

EQUATION

反应方程式

HRID 981437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4-Dimethyl-4-isopropyl-2-oxazolin-5-one (2.0 g) is mixed with DMF (50 mL), THF (70 mL) and sodium p-toluene sulfonamide (5.0 g), and the resulting mixture is heated at reflux for 16 hours. At the end of this time the mixture is cooled, and the solvents are removed under vacuum. The residue is mixed with water and the pH adjusted to 8 with NaHCO3. The aqueous mixture is extracted with ethyl acetate and the organic layers are discarded. The aqueous mixture is acidified to pH-4 with HCl and saturated with NaCl and extracted with ethyl acetate. The organic extracts are combined, dried over MgSO4, filtered and evaporated to give 0.66 of the title product.

WORKUP

后处理

  1. temperaturethe resulting mixture is heated
  2. temperatureat reflux for 16 hours
  3. temperatureAt the end of this time the mixture is cooled
  4. customthe solvents are removed under vacuum
  5. additionThe residue is mixed with water
  6. extractionThe aqueous mixture is extracted with ethyl acetate
  7. extractionextracted with ethyl acetate
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated