HRID1696699

反应详情

EQUATION

反应方程式

HRID 1696699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium tert-butoxide (67.9 g, 605 mmol) was dissolved in a mixed solvent of DMF (500 mL) and THF (500 mL), then with cooling with ice, 2-methoxyphenol (68.28 g, 550 mmol) was dropwise added. This was stirred at room temperature for 2 hours, and then chloromethyl methyl ether (46 mL, 605 mmol) was added. After stirred for 5 hours at room temperature, aqueous saturated ammonium chloride solution was added to the reaction solution, and extracted with ethyl acetate. The organic layer was washed with saturated saline, then dried with sodium sulfate, and concentrated. Purified by silica gel column chromatography, the intended compound (97.66 g, 100%) was obtained as a pale yellow oil.

WORKUP

后处理

  1. additionwas dropwise added
  2. stirringAfter stirred for 5 hours at room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated saline
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated
  7. customPurified by silica gel column chromatography