HRID1666607

反应详情

EQUATION

反应方程式

HRID 1666607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 2-chloro-4-cyclohexylquinazoline (0.25 g), 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (0.49 g), N,N-diisopropylethylamine (0.52 mL), N-methylpyrrolidone (1.0 mL), and n-butanol (1.0 mL) was stirred at 130° C. for 24 h. To the reaction mixture was added saturated aqueous sodium hydrogencarbonate, and the mixture was extracted with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate) to obtain the title compound (0.21 g).

WORKUP

后处理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. customthe desiccant was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate)