反応 #2301439

ord-7be792d34d0f4693ac124f86c25fabc4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was evaporated
  2. 2
    その他the residue was partitioned between water and ether
  3. 3
    抽出extracted with ethyl acetate
  4. 4
    乾燥by drying over sodium sulfate, filtration and evaporation

実験手順

To a solution of the compound of example 65 (2.27 g, 4.39 mmol) in a mixture of methanol/water (4:1, 50 mL) was added a solution of sodium hydroxide (1N, 9 mL). The resulting mixture was stirred for 24 h at room temperature. The solvent was evaporated and the residue was partitioned between water and ether. The alkaline phase acidified using HCl (6N) and extracted with ethyl acetate followed by drying over sodium sulfate, filtration and evaporation. The product was converted to an off-white foam under high vacuum. 1H-NMR(CDCl3, 400 MH: 1.42(s, 9H); 1.59(m, 3H); 1.88–2.54(m, 4H); 7.33(m, 15H); 7.46(s, broad, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07105539B2uspto-grants-2006_09