反応 #90756

ord-592aede79fc24546b0bb8af1b3bc24a1

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was quenched with water
  2. 2
    抽出extracted with EA
  3. 3
    洗浄the combined organic layer was washed with water, brine
  4. 4
    乾燥dried over anhydrous Na2SO4
  5. 5
    濃縮The organic layer was concentrated in vacuo

実験手順

To a solution of 7-(8-chloroimidazo[1,5-a]pyrazin-3-yl)-3-(trifluoromethyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyridine (335 mg, 0.978 mmol) in DMF (4.9 mL) was added NBS (226.19 mg, 1.271 mmol) at ice water, the resulting solution was stirred at this temperature for 10 minutes. The reaction was quenched with water, then extracted with EA and the combined organic layer was washed with water, brine and dried over anhydrous Na2SO4. The organic layer was concentrated in vacuo to give 7-(1-bromo-8-chloroimidazo[1,5-a]pyrazin-3-yl)-3-(trifluoromethyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyridine (0.41 g, yield 99%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09446130B2uspto-grants-2016_09