HRID1704733

反应详情

EQUATION

反应方程式

HRID 1704733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-phenoxy-2-propanol (1 mole) dissolved in pyridine (500 ml) is added methane sulfochloride (1 mole) at a rate sufficient for the temperature of the reaction mixture to reach a value of 40°-50° C., with stirring. On completion of the addition, the reactor is sealed and the reaction mixture is left aside at room temperature during 48 hours. The reaction mixture is then poured over ice. The aqueous phase is extracted with methylene chloride. The organic phase is washed with dilute sulfuric acid and then with water to neutral pH. The resulting material is dried over sodium sulfate and concentrated, to give an oil which crystallizes. The material is taken up into ether, with stirring, to give a white precipitate which is suction filtered. M.p. = 58° C.

WORKUP

后处理

  1. customa value of 40°-50° C.
  2. additionOn completion of the addition
  3. customthe reactor is sealed
  4. additionThe reaction mixture is then poured over ice
  5. extractionThe aqueous phase is extracted with methylene chloride
  6. washThe organic phase is washed with dilute sulfuric acid
  7. dry with materialThe resulting material is dried over sodium sulfate
  8. concentrationconcentrated
  9. customto give an oil which
  10. customcrystallizes
  11. stirringwith stirring
  12. customto give a white precipitate which
  13. filtrationfiltered