HRID1499370

反应详情

EQUATION

反应方程式

HRID 1499370 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oleyl alcohol, also called cis 9 octadecen-1-ol, (100 g, 0.37M) was dissolved in DCM, dichloromethane and cooled to 0° C. Triethylamine (56.5 g, 78 ml, 0.56M, 1.5 equivalents) was added to the solution at this temperature and the mixture was stirred for one hour. Methanesulphonyl chloride (47 g, 31.8 ml, 1.1 equivalents) was then added to the mixture at this temperature and the mixture was stirred at 0° C. for 30 minutes before being allowed to warm to room temperature. The reaction mixture was washed with ice/water, cold 10% hydrochloric acid, cold solution of sodium bicarbonate, water and brine successively, then dried with sodium sulphate. After filtration, the solvent was removed under vacuum to yield and oil which was chilled overnight to yield a solid with a low melting point (yield 126.5 g, 99%).

WORKUP

后处理

  1. stirringthe mixture was stirred at 0° C. for 30 minutes
  2. washThe reaction mixture was washed with ice/water, cold 10% hydrochloric acid, cold solution of sodium bicarbonate, water and brine successively
  3. dry with materialdried with sodium sulphate
  4. filtrationAfter filtration
  5. customthe solvent was removed under vacuum
  6. customto yield
  7. temperatureoil which was chilled overnight
  8. customto yield a solid with a low melting point (yield 126.5 g, 99%)