Hydrochloric Acid → HCID 178453601, Verbindung

HRID 322495Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 322495
[C:1]([O:5][C:6]([NH:8][CH2:9][C@H:10]1[CH2:15][CH2:14][C@H:13]([CH2:16][NH2:17])[CH2:12][CH2:11]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CO.[ClH:20].O1CCOCC1>C(OCC)C>[ClH:20].[C:1]([O:5][C:6]([NH:8][CH2:9][C@H:10]1[CH2:11][CH2:12][C@H:13]([CH2:16][NH2:17])[CH2:14][CH2:15]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 312751,4-DioxaneHCID 178453600HCID 178453600, Verbindung

Produkt 1

HCID 178453601HCID 178453601, VerbindungAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Ethanol (40 mL) was added to N-tert-butoxycarbonyl-trans-4-(aminomethyl)cyclohexanemethyl azide (1.79 g, 6.67 mmol.) and 5% palladium on carbon (270 mg, 0.15 wt. %) under nitrogen. The reaction mixture was stirred under hydrogen at atmospheric pressure for 6 hours at 23° C. The black suspension was filtered and the filtrate concentrated to give N-tert-butoxycarbonyl-trans-1,4-cyclohexane bis(methylamine) as a yellow oil. The crude amine was taken up into methanol (2.0 mL) followed by addition of hydrogen chloride in dioxane (4.0 M, 2.0 mL, 8.0 mmol.) and ethyl ether (25 mL). The resulting precipitate was collected by filtration to give N-tert-butoxycarbonyl-trans-1,4-cyclohexanebis(methylamine) hydrochloride (1.42 g, 76% yield) as a colorless solid.

Aufarbeitung

  1. filtrationThe resulting precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-4cc7202d08ff4f93a056b21ecac02178
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211228B1

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