反応 #86458

ord-66dfde43b4094517a531ba18ffed4f1b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 24 h
  2. 2
    その他The resulting reaction mixture
  3. 3
    濃縮concentrated under vacuum
  4. 4
    その他to get a crude residue
  5. 5
    抽出extracted with ether (3×30 mL)
  6. 6
    ろ過HCl and the precipitated solid was filtered
  7. 7
    洗浄washed with cold water
  8. 8
    その他dried in vacuo

実験手順

A suspension of methyl 2-chloro-6-fluoro-3,5-dimethoxybenzoate (2.7 g, 0.010 mol) and sodium hydroxide (1.088 g, 0.0272) in anhydrous ethanol (30 mL) was refluxed for 24 h. The resulting reaction mixture was cooled to room temperature and concentrated under vacuum to get a crude residue. The crude residue was dissolved in water and extracted with ether (3×30 mL). The aqueous layer was acidified with conc.HCl and the precipitated solid was filtered, washed with cold water and dried in vacuo to afford the title compound (1.8 g, yield: 71%) as a solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434697B2uspto-grants-2016_09