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67705-38-8

6bH-2a,4a,6a-Triazacyclopenta[cd]pentalene, hexahydro- (9Ci) synthesis

6synthesis methods
-

Yield:-

Reaction Conditions:

toluene-4-sulfonic acid at 150;

Steps:



1,4,7-Triazatricyclo[5.2.1.0410]decane (Orthoamide) 0.5 mol 1,4,7-triazacyclononane, 64.3 g, 0.54 mol orthoformicacidtriethylester, 74.8 g, and 20 mmol p-toluolsulphonacid, 4 g, are heated to 150° C. The ethanol that is created and some of the esters are distilled off. After the reaction has been completed the orthoamide can be distilled off at a pressure of <80 mbar in the form of a bright yellow volatile oil (b.p. 350 K at 133 Pa), in agreement with literature (T. J. Atkins, J. Am. Chem. Soc., 102, 6365 (1980)).

References:

US6646122,2003,B1 Location in patent:Page/Page column 7