HRID268119

反应详情

EQUATION

反应方程式

HRID 268119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 100 ml. of ethanol was added 6.2 g. of 5-(3-methyl-2-octyl)resorcinol and 6.2 g. of ethyl 5,5-dimethyl-3-oxotetrahydrothiophene-2-carboxylate. The mixture was cooled in ice and hydrogen chloride was bubbled in for one-half hour. The mixture was stoppered and held at room temperature for 3 days. It was then concentrated and ether added, extracted with water and then washed with dilute aqueous sodium bicarbonate solution. The etheral solution was dried over magnesium sulfate and concentrated. The product was crystallized from acetonitrile to give 5.0 g., m.p. 155°-163°C.

WORKUP

后处理

  1. temperatureThe mixture was cooled in ice
  2. customhydrogen chloride was bubbled in for one-half hour
  3. concentrationIt was then concentrated
  4. additionether added
  5. extractionextracted with water
  6. washwashed with dilute aqueous sodium bicarbonate solution
  7. dry with materialThe etheral solution was dried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe product was crystallized from acetonitrile
  10. customto give 5.0 g