2-Iodohexane → HCID 22923697, Verbindung

HRID 1107565

Reaktionsgleichung

Reaktionsgleichung von HRID 1107565
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.I[CH:9]([CH2:11][CH2:12][CH2:13][CH3:14])[CH3:10]>CC(CC)=O>[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([CH2:10][CH2:9][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:4][CH2:3]1

Komponenten

4

Versuchsvorschrift

4-Hydroxypiperidine (2.02 g, 20 mmol) was dissolved in 100 mL of methyl ethylketone. To this stirred mixture was added 2-iodohexane (1.5 mL, 10 mmol) and the resulting solution was heated at reflux for 1.5 hours. The mixture was allowed to cool and was then washed with saturated aqueous sodium bicarbonate (3×75 mL). The organic layer was dried over magnesium sulfate, filtered, and evaporated, and the residue was dried overnight under house vacuum to yield 1.184 g (64%) of the title compound which was used without further purification. 1H NMR consistent with desired product. MS(FD) 186(M+).

Aufarbeitung

  1. temperaturethe resulting solution was heated
  2. temperatureat reflux for 1.5 hours
  3. temperatureto cool
  4. washwas then washed with saturated aqueous sodium bicarbonate (3×75 mL)
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customthe residue was dried overnight under house vacuum

Quellen und Nachweise

ORD-Eintrag
ord-e3f26c66634643b08fe45bb101c390a3
Quelldatensatz
uspto-grants-2000_05
Patentnummer
US06060488

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