反応式
[H-].[Na+].[C:3]([NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13])(=[O:5])[CH3:4].Cl[CH:15]1[CH2:19][CH2:18][CH:17]=[CH:16]1>CN(C=O)C>[CH:19]1([O:13][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:3](=[O:5])[CH3:4])[CH2:18][CH2:17][CH:16]=[CH:15]1参加物
5
実験手順
To a suspension of sodium hydride (60 proc. in paraffin; 297 mg, 7.43 mmol, 1.1 equiv.) in DMF (3 ml) a solution of 2-acetamido-phenol (1.02 g, 6.75 mmol, 1.0 equiv.) in DMF (12 ml) was added dropwise at 0° C. After 30 minutes chlorocyclopent-2-ene (R. Moffett. Organic Synthesis, Wiley: New York 1963, Collect. Vol. IV, p.238-241) (762 mg, 0.76 ml, 7.43 mmol, 1.1 equiv.) was added by a syringe and stirring was continued overnight. Aqueous work-up followed by flash chromatography on silica gel (heptane/ethyl acetate, 2:1 continued to 1:1) afforded 992 mg (68%) of the subtitle compound as a dark, yellow oil.
後処理
- additionwas added dropwise at 0° C
出典と根拠
- ORDレコード
- ord-65dd917a49504dbab2767eade97d99e2
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06943188B2
関連ノート
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