HRID400621

反应详情

EQUATION

反应方程式

HRID 400621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

A solution of 3-(5-fluoro-2-methylphenyl)-3-methyl-1-morpholin-4-ylbutan-1-one (200 mg, 0.716 mmol) in 2 mL of THF was treated with i-PrLi (0.7 M in pentane, 1.28 mL) at −78° C. The reaction mixture was stirred at −78° C. for 1 hour, allowed to warm to room temperature, quenched with 1 mL of methanol and 5 mL of saturated aqueous ammonium chloride solution, and extracted with three 50 mL portions of ethyl acetate. The combined organic layers were dried over magnesium sulfate, filtered, and concentrated in vacuo. Chromatography on SiO2 (100% hexanes to 25% ethyl acetate in hexanes, gradient) afforded 80.4 mg of the title product (48% yield).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. customquenched with 1 mL of methanol and 5 mL of saturated aqueous ammonium chloride solution
  3. extractionextracted with three 50 mL portions of ethyl acetate
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo