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Glyoxal → cis-Decahydro-2a,4a,6a,8a-tetraazacyclopent[fg]acenaphthylene

HRID 1276094
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Reaktionsgleichung

Reaktionsgleichung von HRID 1276094
[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][NH:10][CH2:11][CH3:12].C(=O)([O-])[O-].[K+].[K+].[CH:19]([CH:21]=O)=O>C(#N)C>[N:10]12[CH:21]3[N:7]([CH2:6][CH2:5][N:4]4[CH:19]3[N:1]([CH2:12][CH2:11]1)[CH2:2][CH2:3]4)[CH2:8][CH2:9]2
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Komponenten

5

Edukt 3

HCID 7860GlyoxalHCID 11430Potassium CarbonateHCID 21716031HCID 21716031, Verbindung

Produkt 1

HCID 9794169cis-Decahydro-2a,4a,6a,8a-tetraazacyclopent[fg]acenaphthylene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1,4,7,10-tetraazadodecane (1.1.4) trihydrobromide in acetonitrile L- 5 with potassium carbonate was reacted with glyoxal to form 1,4,7,10-tetraazatetracyclo-[5,5,2,04,13,010,14 ] tetradecane (1.1.23). Following separation the pure product was obtained by low pressure distillation. This was dissolved in acetonitrile and benzylbromide was added to form 1,7-dibenzylonium-1,4,7,10-tetraazatetracyclo[5,5,2,04,13 010,14 ] tetradecane (1.1.24). Following recrystallization from ethanol this was reacted with sodium borohydride. HCl was added, followed by water and NaOH, and the product extracted with chloroform. Following evaporation of solvent the solids were dissolved in methanol and HBr was added to obtain 1,7-dibenzyl-1,4,7,10-tetraazabicyclo 15.5.2] tetradecane (1.1.25) as the hydrobromide salt. This was dissolved in water and reduced using H2 and a Pd-C catalyst to remove the benzyl groups. Purification of the title compound was by crystallization of the hydrobromide salt. The base form was obtained by low pressure distillation following addition of base. ##STR9##

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ORD-Eintrag
ord-b6e20bb004bf44a89e15d0280f06bbaa
Quelldatensatz
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06165996

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