反応式
Br[CH2:2][C:3](Br)=[O:4].[CH:6]([C:9]1[CH:15]=[CH:14][CH:13]=[C:12]([CH:16]([CH3:18])[CH3:17])[C:10]=1[NH2:11])([CH3:8])[CH3:7].[CH2:19]([NH2:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(N(CC)CC)C>[CH3:17][CH:16]([C:12]1[CH:13]=[CH:14][CH:15]=[C:9]([CH:6]([CH3:8])[CH3:7])[C:10]=1[NH:11][C:3](=[O:4])[CH2:2][NH:26][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:18]参加物
5
実験手順
Bromoacetylbromide (4.5 mL) was added portionwise to a mixture of 8.85 g 2,6-diisopropylaniline and 7.0 mL triethylamine in 300 mL EtoAc at 0° C. Upon completing the addition, excess triethylamine and 5.4 g benzylamine were added and the entire mixture was heated on the steambath for 30 minutes. The reaction mixture was allowed to sit overnight at room temperature, and was then filtered, concentrated, and filtered through silica gel (70-230 mesh) using hexane/EtoAc, 1/1, as eluant. A total of 15.62 g (96%) of the title product was obtained.
後処理
- additionwere added
- temperaturethe entire mixture was heated on the steambath for 30 minutes
- filtrationwas then filtered
- concentrationconcentrated
- filtrationfiltered through silica gel (70-230 mesh)
出典と根拠
- ORDレコード
- ord-6a16c88ba0b2498c9f6d4e1a74c93659
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05153226
関連ノート
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