HRID565631

反应详情

EQUATION

反应方程式

HRID 565631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a reactor equipped with a water trap (Dean-Stark trap), a mixture of benzhydrol (5.0 g), 1-(2-hydroxyethyl)piperazine (3.5 g), camphor-10-sulfonic acid (14 g), and toluene (80 mL) was refluxed for 6 hours. Then, 1N-hydrochloric acid was added and the mixture was separated into two phases. The aqueous layer was made basic with 5 N aqueous sodium hydroxide, saturated with sodium chloride, and extracted with chloroform. The extract was washed with a small amount of saturated aqueous NaCl, dried over MgSO4, and concentrated under reduced pressure to provide 1.9 g of the title compound. Yield 24%. This compound was not further purified but directly submitted to the next reaction.

WORKUP

后处理

  1. customIn a reactor equipped with a water trap (Dean-Stark trap)
  2. temperaturewas refluxed for 6 hours
  3. customthe mixture was separated into two phases
  4. extractionextracted with chloroform
  5. washThe extract was washed with a small amount of saturated aqueous NaCl
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure