HRID916022

反应详情

EQUATION

反应方程式

HRID 916022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the above 3-(5-fluoro-2-methoxyphenyl)-3-methyl-1-morpholin-4-ylbutan-1-one (0.59 g) in THF (1 mL) stirred under argon and cooled on dry ice/acetone was added methyl lithium (1.4 M in pentane, 2 mL) over 2 minutes. The mixture was stirred for 30 minutes and quenched with EtOH (0.3 mL). The mixture was warmed to room temperature and 1 mL of water was added. The organic phase was separated, washed, dried, filtered, and evaporated. The residue was fractionated over a short column of silica gel (eluent:hexanes-methylene chloride (1:1)) to give 4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one as an oil (0.36 g).

WORKUP

后处理

  1. temperaturecooled on dry ice/acetone
  2. customquenched with EtOH (0.3 mL)
  3. addition1 mL of water was added
  4. customThe organic phase was separated
  5. washwashed
  6. customdried
  7. filtrationfiltered
  8. customevaporated