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

HRID 336836

반응식

HRID 336836 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c4556eb69876429c80231218238a6038
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889711B2

연결된 노트

불러오는 중…