HRID484593

反应详情

EQUATION

反应方程式

HRID 484593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-[3-(hydroxymethyl)phenyl]-4-(tetradecyloxy)benzamide and 3.47 g of methanesulfonyl chloride in 200 ml of tetrahydrofuran is added 3.07 g of triethylamine followed by stirring at ambient temperature for 2 hours. Also added is 21.93 g of lithium bromide followed by stirring at ambient temperature for an additional 3 hours. The mixture is poured into water and extracted with ether. The organic layer is washed with a mixture of brine and saturated sodium bicarbonate then dried. The solvent is removed under vacuum and the residue crystallized from carbon tetrachloride:hexanes to give the desired product as a white solid, m.p. 116°-118° C.

WORKUP

后处理

  1. additionAlso added
  2. stirringby stirring at ambient temperature for an additional 3 hours
  3. extractionextracted with ether
  4. washThe organic layer is washed with a mixture of brine and saturated sodium bicarbonate
  5. customthen dried
  6. customThe solvent is removed under vacuum
  7. customthe residue crystallized from carbon tetrachloride