反応 #217158

ord-d4e7992cdae44a089019052663980c8b

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他solvent was removed in-vacuo
  2. 2
    workup.ADDITIONthe residue treated with 1 ml of water
  3. 3
    抽出extracted with 1×3 ml portions of ether
  4. 4
    抽出extracted with 3×3 ml portions of ether
  5. 5
    乾燥Combined ether extracts were dried (MgSO4)
  6. 6
    濃縮concentrated in-vacuo

実験手順

To a stirred solution of 0.130 g (0.38 mmol) of ethyl-6-[2-(2,6,6-trimethyl-cyclohex-1-enyl)-ethynyl]2-naphthoate (Compound 2) in 0.7 ml of ethanol was added dropwise under nitrogen 0.9 ml of a 1.86M solution of KOH in ethanol and water. After being stirred at 50 degrees C. for 18 hours, solvent was removed in-vacuo and the residue treated with 1 ml of water and extracted with 1×3 ml portions of ether. The aqueous layer was then acidified with dilute HCl and extracted with 3×3 ml portions of ether. Combined ether extracts were dried (MgSO4) and concentrated in-vacuo to give the title product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05470999uspto-grants-1995_11