HRID1291196
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionThen, 100 ml of 1N aqueous HCI were added
- stirringthe mixture was stirred for 5 min.
- washthe organic phase was washed with 1N aqueous HCI, with saturated bicarbonate solution and with saturated sodium chloride solution
- dry with materialdried over sodium sulfate