反応 #2275727

ord-9ab9905baa1c470ca236d29b40e48295

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed in vacuo and residue
  2. 2
    その他partitioned between ethyl acetate and water
  3. 3
    洗浄The organic layer was washed with brine
  4. 4
    乾燥dried over anhydrous Na2SO4
  5. 5
    ろ過filtered
  6. 6
    濃縮concentrated

実験手順

A solution of 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-pyridin-2-one (as prepared in the previous step, ˜300 mg, 1.28 mmol)) in acetone (10 mL) was treated with 1N HCl (2 mL) at room temperature for 4 hours. The reaction was worked up with saturated sodium bicarbonate to adjust the pH to neutral. The solvent was removed in vacuo and residue partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, concentrated to afford the title compound as white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08324186B2uspto-grants-2012_12