反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[NH:6][CH3:7])#[CH:2].Br[C:12]#[C:13][C:14]([OH:17])([CH3:16])[CH3:15]>C(N)(C)C.CO.[Cu]Cl>[OH:17][C:14]([CH3:16])([CH3:15])[C:13]#[C:12][C:2]#[C:1][C:3]1[CH:10]=[CH:9][CH:8]=[C:5]([NH:6][CH3:7])[CH:4]=1参加物
実験手順
100 mg of copper (I) chloride were dissolved in a mixture of 20 ml of isopropylamine and 10 ml of methanol in an atmosphere of argon, and 1350 mg of 3-ethynyl-N-methylaniline were then added to the reaction mixture, followed by stirring at room temperature for 10 minutes. 3300 mg of 1-bromo-3-hydroxy-3-methyl-1-butyne were then dropwisely added to the solution over a time of about 3 hours, followed by stirring at room temperature for 2 hours. After the solvent had been evaporated from the reaction mixture, the residue was neutralized and diluted by 1N hydrochloric acid and subjected to extraction with 50 ml of ether three times. The organic layer was dried over magnesium sulfate, and the solvent was then evaporated. The residue was then purified by silica-gel chromatography using benzene as an eluent to obtain 1600 mg of 5-hydroxy-5-methyl-1-[3-(N-methylamino)phenyl] hexa-1,3-diyne.
後処理
- additionwere then added to the reaction mixture
- stirringby stirring at room temperature for 2 hours
- customAfter the solvent had been evaporated from the reaction mixture
- additiondiluted by 1N hydrochloric acid
- extractionsubjected to extraction with 50 ml of ether three times
- dry with materialThe organic layer was dried over magnesium sulfate
- customthe solvent was then evaporated
- customThe residue was then purified by silica-gel chromatography
出典と根拠
- ORDレコード
- ord-215e1af49e9c454d834c4837b45a4e8f
- 出典データセット
- uspto-grants-1993_03
- 特許番号
- US05196586
関連ノート
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