反応式
[Br:1]Br.[C:3]([C:6]1[CH:7]=[C:8]([C:24]([NH:26][CH2:27][C:28]2[CH:33]=[CH:32][C:31]([S:34]([CH3:37])(=[O:36])=[O:35])=[CH:30][CH:29]=2)=[O:25])[C:9](=[O:23])[N:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=2)[C:11]=1[CH3:12])(=[O:5])[CH3:4]>C1COCC1>[Br:1][CH2:4][C:3]([C:6]1[CH:7]=[C:8]([C:24]([NH:26][CH2:27][C:28]2[CH:33]=[CH:32][C:31]([S:34]([CH3:37])(=[O:36])=[O:35])=[CH:30][CH:29]=2)=[O:25])[C:9](=[O:23])[N:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=2)[C:11]=1[CH3:12])=[O:5]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
Bromine (34 μl, 0.66 mmol) in THF (5 ml) was added to a solution of 5-acetyl-6-methyl-N-[4-(methylsulfonyl)benzyl]-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxamide (320 mg, 0.63 mmol) in TBF (10 ml). After 2 h, the yellow colour had disappeared. The reaction mixture was partitioned between water and ethyl acetate, the organic phase was separated, evaporated, and the residue was chromatographed on silica using ethyl acetate/heptane (1/1, 2/1, 4/1) as eluent. Fractions containing the product were combined and evaporated to give the title compound (150 mg, 41%).
後処理
- customThe reaction mixture was partitioned between water and ethyl acetate
- customthe organic phase was separated
- customevaporated
- customthe residue was chromatographed on silica
- additionFractions containing the product
- customevaporated
出典と根拠
- ORDレコード
- ord-dbd44ed61af040a1a5ed792afd81e0c5
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063073B2
関連ノート
読み込み中…