反応 #319201

ord-aa7a8ecdaee24c5096f3066089c40040

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他has formed
  2. 2
    温度The solution is cooled
  3. 3
    洗浄washed with 200 ml of methylene chloride
  4. 4
    抽出extracted several times with methylene chloride
  5. 5
    その他the extract is dried
  6. 6
    その他evaporated down
  7. 7
    その他to give a colorless residue which
  8. 8
    その他crystallizes spontaneously

実験手順

151 g of the above product from (a) are stirred with 650 ml of 2N sodium hydroxide solution at 90° C. until a clear solution has formed. The solution is cooled and then washed with 200 ml of methylene chloride, the aqueous phase is acidified with concentrated hydrochloric acid and extracted several times with methylene chloride, and the extract is dried and evaporated down to give a colorless residue which crystallizes spontaneously. Yield: 129 g (88% of theory, based on methyl 1-hydroxypyrazole-4-carboxylate). M.p.: 85° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04851410uspto-grants-1989_07