HRID732243

反应详情

EQUATION

反应方程式

HRID 732243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While 77.0 g of 2-bromo-1-(4-methoxy-phenyl)-3-methyl-butan-1-one (4) prepared in Example 2 were added to 200 ml of ethanol and stirred, 42.7 g of thioacetamide were added. Subsequently, the temperature was gradually increased and stirring under reflux was continued for 22 hr. After the reaction was completed, the resultant reaction mixture was added with 300 ml of ethylacetate, and then washed with a saturated aqueous solution of potassium carbonate. The ethylacetate layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure, thus obtaining 35.8 g (yield: 51.0%) of a title compound as brown liquid.

WORKUP

后处理

  1. temperatureSubsequently, the temperature was gradually increased
  2. stirringstirring
  3. temperatureunder reflux
  4. customthe resultant reaction mixture
  5. washwashed with a saturated aqueous solution of potassium carbonate
  6. dry with materialThe ethylacetate layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure