1-Bromooctane → HCID 20322535, Verbindung

HRID 840003Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 840003
[K].[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[NH:8][C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3].[CH2:21](Br)[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>CN(C)C=O>[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[N:8]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3]

Komponenten

5

Edukt 3

HCID 81401-BromooctaneHCID 5462222PotassiumHCID 203401897,9-Diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione2×

Produkt 1

HCID 20322535HCID 20322535, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To 70 ml of dimethylformamide were added 8 g of the potassium salt of 7,9-diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione (Compound 1) and 5.2 g of octyl bromide; the mixture was heated, with stirring, at 60° C for 2 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and benzene was added to the residue. The resulting benzene solution was washed with water and then dried over magnesium sulphate. After removing the benzene, the resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine) and then by recrystallization from hexane, giving 3.0 g of Compound 5, mp 65° - 67° C.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure, and benzene
  3. additionwas added to the residue
  4. washThe resulting benzene solution was washed with water
  5. dry with materialdried over magnesium sulphate
  6. customAfter removing the benzene
  7. customthe resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine)
  8. customby recrystallization from hexane

Quellen und Nachweise

ORD-Eintrag
ord-a113adb3b1af40ceb38cfcd397f3a084
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04097587

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