反応 #80080

ord-006600b3e266453f83e57eab17a675f9

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution was cooled to room temperature
  2. 2
    濃縮concentrated under reduced pressure

実験手順

A solution of imidazole (58.0 mg, 0.86 mmol) in 3 mL DMF was treated with NaH (20.0 mg, 0.86 mmol) and heated to 90° C. After 1 h a solution of 4-bromo-1-bromomethyl-2-methyl-benzene (Intermediate 138, 190.0 mg, 0.72 mmol) in 3 mL DMF was added and stirring at 90° C. continued for 1 hour. The solution was cooled to room temperature and concentrated under reduced pressure. The title compound, 160.0 mg (88%) was isolated by column chromatography (5% MeOH-EtOAc) as a colorless solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713647B2uspto-grants-2004_03