反応式
[OH:1][C:2]1[C:10]2[O:9][C:8]([C:11]([C:13]3[C:14]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[N:15][O:16][C:17]=3[CH3:18])=[O:12])=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.Cl[CH2:26][C:27]([NH:29][CH:30]([CH3:32])[CH3:31])=[O:28].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH:30]([NH:29][C:27](=[O:28])[CH2:26][O:1][C:2]1[C:10]2[O:9][C:8]([C:11]([C:13]3[C:14]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[N:15][O:16][C:17]=3[CH3:18])=[O:12])=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1)([CH3:32])[CH3:31]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of (7-hydroxy-2-benzofuranyl)(5-methyl-3-phenyl-4-isoxazolyl)methanone (example 4) (100 mg, 0.31 mmol) in DMF (5 mL) was added N-(chloroacetyl)isopropylamine (47 mg, 0.34 mmol) and potassium carbonate (173 mg, 1.25 mmol) and the reaction mixture was stirred at room temperature for 4 h. The mixture was then poured onto ice-water, and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over Na2SO4 and evaporated. Purification by chromatography (SiO2, heptane:ethyl acetate:=100:0 to 1:1) afforded the title compound (37 mg, 28%) as a white solid. MS m/e: 419.3 [M+H]+.
後処理
- additionThe mixture was then poured onto ice-water
- extractionextracted with ethyl acetate
- washThe combined organic layers were then washed with water and brine
- dry with materialdried over Na2SO4
- customevaporated
- customPurification by chromatography (SiO2, heptane:ethyl acetate:=100:0 to 1:1)
出典と根拠
- ORDレコード
- ord-950d29591c214990904ac7f450664db7
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07388025B2
関連ノート
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