HRID1820301

反应详情

EQUATION

反应方程式

HRID 1820301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(5-methylpyridin-2-yl)aminopiperidine (394 mg, 2 mmol), sodium hydrogencarbonate (277 mg, 3.2 mmol) and 3-cyclohexyl-3-hydroxypropyl 4-bromobenzenesulfonate (932 mg, 2.4 mmol) in 1,2-dimethoxyethane (10 mL) was refluxed for 8 hours. After then adding 5 g of NH silica Chromatorex DM1020 to the reaction mixture, it was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (60 g NH silica Chromatorex DM2035, hexane:ethyl acetate=1:1) to obtain the title compound as a light yellow solid (405 mg) (59.6% yield).

WORKUP

后处理

  1. temperaturewas refluxed for 8 hours
  2. additionAfter then adding 5 g of NH silica Chromatorex DM1020 to the reaction mixture, it
  3. concentrationwas concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (60 g NH silica Chromatorex DM2035, hexane:ethyl acetate=1:1)