HRID916024

反应详情

EQUATION

反应方程式

HRID 916024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

To a solution of cyclohexylmethyl bromide (0.26 g) in THF (1 mL) cooled to −70° C. under argon, tert-butyl lithium (1.7 M in pentane, 1.8 mL) was added dropwise over 5 minutes. The mixture was stirred at −70° C. for 30 minutes. A solution of 3-(5-fluoro-2-methoxyphenyl)-3-methyl-1-morpholin-4-ylbutan-1-one (0.33 g) in THF (1 mL) was added all at once and the mixture was stirred for one hour. The reaction temperature rose to approximately −20° C. The reaction was quenched with EtOH (0.3 mL) and warmed to room temperature. The mixture was diluted with EtOAc, washed with water, dried, filtered, and evaporated. Chromatography of the residue over silica gel (eluent:hexanes to methylene chloride gradient) gave the title compound as an oil (0.2 g).

WORKUP

后处理

  1. stirringwas stirred for one hour
  2. customrose to approximately −20° C
  3. customThe reaction was quenched with EtOH (0.3 mL)
  4. temperaturewarmed to room temperature
  5. additionThe mixture was diluted with EtOAc
  6. washwashed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated