HRID1669328

反应详情

EQUATION

反应方程式

HRID 1669328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Bromo-N-methoxy-3,N-dimethyl-benzamide (5.94 g, 23.05 mmol) was suspended in anhydrous tetrahydrofuran (200 mL), and cooled to 0° C. with stirring under nitrogen. 1-magnesium bromo-4-methyl-pentane (23 mL, 1.5M in tetrahydrofuran, 34.8 mmol) was slowly added to the reaction over 1 h. The reaction was allowed to warm slowly to room temperature and monitored by TLC. Upon complete consumption of starting material, the reaction was carefully neutralized with 1N hydrochloric acid, extracted with diethyl ether, washed, dried, and concentrated. The 1-(4-Bromo-3-methyl-phenyl)-5-methyl-hexan-1-one (5.2 g, 18.4 mmol) 80% yield, was used without further purification.

WORKUP

后处理

  1. temperatureto warm slowly to room temperature
  2. customUpon complete consumption of starting material
  3. extractionextracted with diethyl ether
  4. washwashed
  5. customdried
  6. concentrationconcentrated