HRID55598

反应详情

EQUATION

反应方程式

HRID 55598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-[2-(3-hydroxypropoxy)phenyl]-acetamide (Example 113) (7.5 g, 36 mmol) in pyridine (90 ml), cooled to 0° C., was added p-toluenesulfonyl chloride (13.6 g, 56 mmol). After the tosyl chloride went into solution, the reaction was then allowed to stand at 5° C. for 16 hours. The reaction was poured onto ice, and a brown oil settled. The aqueous supernatant was decanted from the oil, and the residual oil taken up in diethyl ether. The diethyl ether was washed with cold (5° C.) 3N HCl and then with brine. The organic layer was dried (MgSO4), and concentrated to afford a thick, brown oil, 5.3 g.

WORKUP

后处理

  1. additionThe reaction was poured onto ice
  2. customThe aqueous supernatant was decanted from the oil
  3. washThe diethyl ether was washed with cold (5° C.) 3N HCl
  4. dry with materialThe organic layer was dried (MgSO4)
  5. concentrationconcentrated
  6. customto afford a thick, brown oil, 5.3 g