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Sodium Iodide → HCID 21409856, 화합물

HRID 2072009
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HRID 2072009 반응식
[CH3:1][NH:2][C:3]([CH3:15])([CH3:14])[CH2:4][NH:5][C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.BrC[CH:18]=[C:19]([CH3:21])[CH3:20].[C:22](=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>CC(CC)=O>[CH3:14][C:3]([N:2]([CH3:22])[CH2:1][CH:18]=[C:19]([CH3:21])[CH3:20])([CH3:15])[CH2:4][NH:5][C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
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HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 21409819N-[2-Methylamino-2-methylpropyl]benzamide

생성물 1

HCID 21409856HCID 21409856, 화합물수율 84.1%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone
용매
2회

실험 절차

A solution of N[2-methylamino-2-methylpropyl] benzamide (1 g., 0.0052 mole) in methylethyl ketone (MEK) (25 ml.) was added to a solution of 1-bromo-3-methyl-but-2-ene (0.78 g., 0.0052 mole) in MEK (40 ml.) containing sodium carbonate (0.55 g., 0.0052 mole) and a few crystals of sodium iodide. The mixture was heated under reflux for 30 hrs. The inorganic solids were filtered off and the filtrant concentrated by evaporation under reduced pressure to give a liquid residue. This was loaded onto an alumina column and eluted with ethyl acetate. Fractions (25 mls) were collected and concentrated to give N[2-methyl-2[methyl(3-methyl-2-butenyl)amino]propyl]benzamide (1.2 g.).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 hrs
  3. filtrationThe inorganic solids were filtered off
  4. concentrationthe filtrant concentrated by evaporation under reduced pressure
  5. customto give a liquid residue
  6. washeluted with ethyl acetate
  7. customFractions (25 mls) were collected
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a410465cd8334cfab880f8ce9c025d67
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04049663

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