HRID2200785

反应详情

EQUATION

反应方程式

HRID 2200785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 mol of sodium hydride was added to the solvent ethylene glycol dimethyl ether, and 1 mol of methyl 4-methoxybutanoate was added thereto and stirred at room temperature for 10 minutes. Then, 1.2 mol of t-butylmethylketone was added to the solution which was then stirred at 92° C. for 19 hours. Then, the solution was cooled to room temperature and quenched in 36% hydrochloric acid, after which water and dimethylether were added to and mixed with the solution, and water was removed therefrom. The resulting organic material was washed with 1 wt % sodium hydroxide and then with saturated saline and concentrated, and the residue was fractionated, thereby obtaining the intermediate 8-methoxy-2,2-dimethyloctan-3,5-dione at a yield of 14%.

WORKUP

后处理

  1. additionwas added
  2. stirringwas then stirred at 92° C. for 19 hours
  3. temperatureThen, the solution was cooled to room temperature
  4. customquenched in 36% hydrochloric acid
  5. additionafter which water and dimethylether were added to and
  6. additionmixed with the solution, and water
  7. customwas removed
  8. washThe resulting organic material was washed with 1 wt % sodium hydroxide
  9. concentrationwith saturated saline and concentrated