1-Methylpiperazine → 5-((4-Methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde

HRID 336836

反応式

HRID 336836 の反応式
Br[CH2:2][C:3]1[O:7][C:6]([CH:8]=[O:9])=[CH:5][CH:4]=1.[CH3:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1>O1CCOCC1>[CH3:10][N:11]1[CH2:16][CH2:15][N:14]([CH2:2][C:3]2[O:7][C:6]([CH:8]=[O:9])=[CH:5][CH:4]=2)[CH2:13][CH2:12]1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 119704915-(Bromomethyl)-2-furaldehyde

生成物 1

HCID 866713815-((4-Methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde収率 55%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 0.20 g (1.1 mmol) of 5-(bromomethyl)furan-2-carboxaldehyde in anhydrous dioxane (10 ml) are added 261 μL (0.24 g, 2.3 mmol) of 1-methylpiperazine. The mixture is stirred at room temperature for 30 min. The precipitate formed is filtered and rinsed with dioxane. The filtrate is concentrated, dissolved in dichloromethane, and washed in water. The organic phase is dried over magnesium sulfate, filtered, and concentrated. The residue obtained is purified by chromatography on silica (eluent: 7N NH4OH in MeOH/CH2Cl2, 5:95) to yield 0.12 g (55%) of 5-((4-methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde in the form of an orange solid.

後処理

  1. customThe precipitate formed
  2. filtrationis filtered
  3. washrinsed with dioxane
  4. concentrationThe filtrate is concentrated
  5. dissolutiondissolved in dichloromethane
  6. washwashed in water
  7. dry with materialThe organic phase is dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe residue obtained
  11. customis purified by chromatography on silica (eluent: 7N NH4OH in MeOH/CH2Cl2, 5:95)

出典と根拠

ORDレコード
ord-c4556eb69876429c80231218238a6038
出典データセット
uspto-grants-2014_11
特許番号
US08889711B2

関連ノート

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