HRID1389397

反应详情

EQUATION

反应方程式

HRID 1389397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7 Grams of methyl 2,6-dimethylphenoxyacetate, 3.4 ml of acetic anhydride and 100 ml of carbon disulfide were mixed at 0° C., and to the mixture was added 17.9 g of aluminum chloride, and the resulting mixture was heated until gas was evolved. After the gas-evolution was ceased, the reaction mixture was refluxed for 30 minutes under heating. Then water was added to the solution. The resulting mixture was extracted with di-isopropyl ether, washed with water, dried over anhydrous magnesium sulfate. The oily solution was concentrated to obtain an oily substance. The oily substance was chromatographed on silica gel to obtain 6.1 g of methyl 4-acetyl-2,6-dimethylphenoxyacetate, nD21.6 1.5165.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated until gas
  2. temperaturethe reaction mixture was refluxed for 30 minutes
  3. temperatureunder heating
  4. extractionThe resulting mixture was extracted with di-isopropyl ether
  5. washwashed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe oily solution was concentrated
  8. customto obtain an oily substance
  9. customThe oily substance was chromatographed on silica gel