7-Bromo-1-Chloroisoquinoline → 7-bromo-N-butyl-N-methylisoquinolin-1-amine
反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[C:9]2Cl)=[CH:4][CH:3]=1>CNCCCC>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[C:9]2[N:8]([CH2:7][CH2:6][CH2:5][CH3:4])[CH3:9])=[CH:4][CH:3]=1参加物
3
実験手順
A solution of 7-bromo-1-chloroisoquinoline (750 mg, 3.09 mmol) in N-methylbutylamine (7.0 mL) was heated at 65° C. in a sealed tube for 18 h. The reaction mixture was concentrated under reduced pressure. The residue was diluted with chloroform and washed with saturated sodium bicarbonate, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield a brown oil. Purification by flash column chromatography (silica, 3:1 hexanes/diethyl ether) provided 7-bromo-N-butyl-N-methylisoquinolin-1-amine (730 mg): ESI MS m/z 293 [M+H]+.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionThe residue was diluted with chloroform
- washwashed with saturated sodium bicarbonate
- dry with materialdried (sodium sulfate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto yield a brown oil
- customPurification by flash column chromatography (silica, 3:1 hexanes/diethyl ether)
出典と根拠
- ORDレコード
- ord-d676ac49f1b945c79fc6cf197f9470f2
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07727997B2
反応ノート
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