HRID1383455

反应详情

EQUATION

反应方程式

HRID 1383455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a round bottom flask, benzhydrol (1.84 g, 10 mmol, 1.0 eq.), piperidin-4-yl-methanol (1.15 g, 10 mmol, 1.0 eq.), and p-toluenesulfonic acid monohydrate (2.09 g, 1.1 eq.) were suspended in toluene (400 ml). The mixture was refluxed with a Dean-Stark condenser for 3-4 hours. After cooling to room temperature, the solution was washed with 5% NaOH solution (2×20 ml), then with water (2×20 ml). The solution was then dried over anhydrous Na2SO4. The solvent was then removed under vacuum. The crude product 4-(1,1-diphenyl-methoxymethyl)-piperidine was obtained (2.33 g, 82.8% yield). ESMS 268.1 (M+1), 290.1 (M+23).

WORKUP

后处理

  1. temperatureThe mixture was refluxed with a Dean-Stark condenser for 3-4 hours
  2. washthe solution was washed with 5% NaOH solution (2×20 ml)
  3. dry with materialThe solution was then dried over anhydrous Na2SO4
  4. customThe solvent was then removed under vacuum