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ChemicalBook CAS DataBase List 1,4,7-Triazacyclononane
4730-54-5

1,4,7-Triazacyclononane synthesis

6synthesis methods
The ligand is prepared from diethylene triamine as follows by macrocyclization using ethyleneglycol ditosylate.
H2NCH2CH2NHCH2CH2NH2 + 3 TsCl → Ts(H)NCH2CH2N(Ts)CH2CHH2N(H)Ts + 3 HCl Ts(H)NCH2CH2N(Ts)CH2CH2N(H)Ts + 2 NaOEt → Ts(Na)NCH2CH2N(Ts)CH2CH2N(Na)Ts Ts(Na)NCHH2CH2N(Ts)CH2CH2N(Na)Ts + TsOCH2CH2OTs + → [(CH2CH2N(Ts)]3 + 2 NaOTs [(CH2CH2N(Ts)]3 + 3 H2O → [CH2CH2NH]3 + 3 HOTs
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Yield:4730-54-5 100%

Reaction Conditions:

with methanol;palladium 10% on activated carbon at 50; for 3 h;

Steps:

1 Synthesis of 1,4,7-triazacyclononane:
1,4,7-Tribenzyl-1,4,7-triazacyclononane (100 mg, 0.25 mmol) was dissolved in 15 mL of methanol.Add 10% Pd/C (100mg),After the reaction was placed at 50 ° C for 3 h,After filtration, Pd/C is removed.The solvent was removed under reduced pressure.Obtained 32 mg of product,The yield was 100%.

References:

Capital University of Medical Sciences;Wu Zehui;Liu Yajing;Huang Yong;Liu Song;Wu Renbo CN108276353, 2018, A Location in patent:Paragraph 0052; 0056; 0063; 0064; 0065

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