HRID1176630

反应详情

EQUATION

反应方程式

HRID 1176630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

0.090 g of benzyl 4-(4-benzyloxyphenyl)-3-[4-(3-methoxypropyl)-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethoxy]piperidine-1-carboxylate is dissolved in 3 ml of dioxane. 3 ml each of methanol and 40% KOH are added and the reaction mixture is stirred in a sealed flask at 100° C. over 3.5 hours. The reaction mixture is subsequently cooled to room temperature, diluted with 10 ml of water and extracted with tert-butyl methyl ether (3×30 ml). The combined organic phases are washed with 10 ml of water, then 10 ml of brine, dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F).

WORKUP

后处理

  1. temperatureThe reaction mixture is subsequently cooled to room temperature
  2. extractionextracted with tert-butyl methyl ether (3×30 ml)
  3. washThe combined organic phases are washed with 10 ml of water
  4. dry with material10 ml of brine, dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation