HRID1291196

反应详情

EQUATION

反应方程式

HRID 1291196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.5 g (0.0342 mol) of 1-benzoyl-4-hydroxymethyl-piperidine were dissolved in 170 ml of dichlormethane and 17 ml (0.122 mol) of triethylamine, cooled to 0° and treated with a solution of 3.14 ml (0.0404 mol) of methanesulfonyl chloride in 20 ml of dichloromethane. The mixture was stirred at 0° for 1/2 hr. Then, 100 ml of 1N aqueous HCI were added, the mixture was stirred for 5 min., the organic phase was washed with 1N aqueous HCI, with saturated bicarbonate solution and with saturated sodium chloride solution and dried over sodium sulfate. 10.2 g (100%) of 1-benzoylpiperidin-4-ylmethyl methanesulfonate were obtained as yellow crystals; m.p. 87°-90°.

WORKUP

后处理

  1. additionThen, 100 ml of 1N aqueous HCI were added
  2. stirringthe mixture was stirred for 5 min.
  3. washthe organic phase was washed with 1N aqueous HCI, with saturated bicarbonate solution and with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate