反応 #89279

ord-dac80aaa1eac40c39c5b1e78352c0f96

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The resulting mixture was extracted with DCM
  2. 2
    洗浄washed with brine
  3. 3
    乾燥dried (MgSO4)
  4. 4
    その他The solvent was removed in vacuo
  5. 5
    その他The crude was purified by silica gel chromatography (EtOAc/hexanes)

実験手順

A solution of 5-bromo-2-methylpyridine (10 g, 58.13 mmol) and meta-chloroperbenzoic acid (mCPBA, 30 g, 174.39 mmol) in CHCl3 (160 mL) was heated at 60° C. for 16 h. The mixture was cooled to rt and neutralized with satd. NaHCO3. The resulting mixture was extracted with DCM. The organic layers were combined and washed with brine and dried (MgSO4). The solvent was removed in vacuo. The crude was purified by silica gel chromatography (EtOAc/hexanes) to obtain the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09440982B2uspto-grants-2016_09