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ChemicalBook CAS DataBase List 1,6-Bis(cyano-guanidino)hexane
15894-70-9

1,6-Bis(cyano-guanidino)hexane synthesis

2synthesis methods
-

Yield:15894-70-9 80%

Reaction Conditions:

in butan-1-ol for 8 h;Reflux;

Steps:

11 1,6-Di-(N3-cyano-N1-guanidino)hexane
A solution of 3.78 g (20.0 mmol, 1 equiv) 1,6-hexamethylenediamine dihydrochloride and 3.56 g (40.0 mmol, 2 equiv) sodium dicyanamide in 28 mL n-butanol was heated to reflux for 8 h.
After cooling to room temperature, the solid was filtered off and washed with butanol and cold water.
Recrystallization from water afforded pure compound 3. Yield: 80%.
Melting point: 195 °C (Ref.: 202-203 °C).
1
1H NMR (300 MHz, [D6]DMSO): δ = 1.23 (m, 4H), 1.39 (m, 4H), 3.02 (m, 4H), 6.63-6.83 (m, 6H) ppm; 13C NMR (100 MHz, [D6]DMSO): δ = 25.9, 28.9, 40.8, 118.4, 161.2 ppm; IR (KBr): = 3372 (s), 3159 (s), 2940 (s), 2940 (m), 2857 (m), 2172 (s), 1650 (s), 1625 (s), 1475 (m), 1439 (s), 1383 (m), 1322 (m), 1128 (m), 928 (w), 733 (w), 689 (w), 561 (m), 541 cm-1 (m); ESI-MS C10H18N8 calcd: 249.2 [M-H+], found: 249.3.

References:

Gr?st, Corinna;Gr?ber, Martin;Hell, Michael;Berg, Thorsten [Bioorganic and Medicinal Chemistry,2013,vol. 21,# 23,p. 7357 - 7363]

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