8-Methylimidazo(1,2-a)pyridine → 8-Methyl-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine
反応式
[CH3:1][C:2]1[C:3]2[N:4]([CH:8]=[CH:9][N:10]=2)[CH:5]=[CH:6][CH:7]=1>C(O)CCC.[Ni]>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]2[CH:8]=[CH:9][N:10]=[C:3]12参加物
4
反応条件
- 温度
- 65 °C
実験手順
1 g of 8-methylimidazo[1,2-a]pyridine [3-1] was dissolved in 20 mL of 1-butanol, and a catalytic amount of Raney nickel of was added thereto. The mixture was stirred under a hydrogen atmosphere (5 atmospheric pressure) at 65° C. for 4 days. After cooling the reaction mixture back to room temperature, the insolubles were filtered through celite, and washed with methanol. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography, to obtain 823.3 mg of 8-methyl-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine [46-1].
後処理
- temperatureAfter cooling the reaction mixture back to room temperature
- filtrationthe insolubles were filtered through celite
- washwashed with methanol
- concentrationThe filtrate was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-8f3eeb8f5b18457c8a4ed2edf6b5570b
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07718801B2
反応ノート
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