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
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
- stirringwas stirred for one hour
- customrose to approximately −20° C
- customThe reaction was quenched with EtOH (0.3 mL)
- temperaturewarmed to room temperature
- additionThe mixture was diluted with EtOAc
- washwashed with water
- customdried
- filtrationfiltered
- customevaporated