Hydrochloric Acid → HCID 12508676, Verbindung

HRID 1633331Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1633331
[CH2:1]([C:6]1([CH3:18])[CH:11]([CH2:12][CH3:13])[NH:10]C(CC)[NH:8][CH:7]1[CH2:16][CH3:17])[NH:2][CH2:3][CH2:4][CH3:5].Cl>O>[NH2:8][CH:7]([CH2:16][CH3:17])[C:6]([CH:11]([NH2:10])[CH2:12][CH3:13])([CH3:18])[CH2:1][NH:2][CH2:3][CH2:4][CH3:5]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 12508669HCID 12508669, Verbindung

Produkt 1

HCID 12508676HCID 12508676, VerbindungAusbeute 84,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 21.1 grams of 5-(2-azapentyl)-5-methyl-2,4,6-triethylhexahydropyrimidine, prepared as described in example 1, 25 grams of conc. HCl and 25 grams of water was refluxed for 2 hours. The organic layer which separated was removed and discarded and the aqueous solution after extraction with ether was basified with a sodium hydroxide solution. The organic layer which separated was removed and the aqueous phase extracted with ether. The ethereal solution was combined with the organic layer and after drying evaporated under diminished pressure to yield 15.0 grams of 7-amino-6-(1-aminopropyl)-6-methyl-4-azanonane; b.p. 72°-76° C./0.05 torr; Infrared spectrum, 2.97 and 3.05μ (N-H) and 6.15μ (NH2); 'H nuclear magnetic resonance spectrum, solvent CDCl3, internal reference tetramethylsilane, δ in ppm: 3.07-2.30, 6H; 2.00-1.14, 6H; 1.14-0.67, 12H. 13C nuclear magnetic resonance spectrum, solvent CDCl3, internal reference tetramethylsilane, δ in ppm: ##STR7## 11.9(1); 23.2(2); 52.9 and 52.8(3); 54.7 and 54.3(5); 42.9 and 43.1(6); 58.8, 56.7 and 57.5(7,11); 24.9, 24.7 and 25.7(8,12); 12.2(9,13); 19.2 and 17.0(10).

Aufarbeitung

  1. customprepared
  2. temperaturewas refluxed for 2 hours
  3. customThe organic layer which separated
  4. customwas removed
  5. extractionthe aqueous solution after extraction with ether
  6. customThe organic layer which separated
  7. customwas removed
  8. extractionthe aqueous phase extracted with ether
  9. customafter drying
  10. customevaporated under diminished pressure

Quellen und Nachweise

ORD-Eintrag
ord-ac4d271be91246adbf866109c4661d80
Quelldatensatz
uspto-grants-1984_10
Patentnummer
US04480095

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