反応 #8501

ord-817f567d751f49859e698e37d51e69b5

反応条件

温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was cooled down to room temperature
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    その他The aqueous layer was separated
  4. 4
    workup.ADDITIONwas added
  5. 5
    workup.STIRRINGwith stirring
  6. 6
    ろ過The obtained slurry was filtered
  7. 7
    洗浄washed with cold water
  8. 8
    その他dried

実験手順

The compound (5) (20.0 g, 62.2 mmol) was suspended in 35% aqueous hydrochloric acid (100 ml). The solution was heated at 85° C. and stirred for 1 hour. The reaction mixture was cooled down to room temperature and water (100 ml) and toluene (44 ml) were added thereto with stirring. The aqueous layer was separated and neutralized with 30% aqueous sodium hydroxide, to which ethyl acetate (30 ml) was added with stirring. The obtained slurry was filtered, washed with cold water and dried to yield 2-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole (9) (11.7 g). Yield 81.4%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087764B2uspto-grants-2006_08