Technology Process of tri-tert-butyl 10-(2-((4-methoxy-3,5-bis(methylcarbamoyl)benzyl)amino)-2-oxoethyl)-1,4,7,10-tetraazacyclododecane-1,4,7-tricarboxylate
There total 8 articles about tri-tert-butyl 10-(2-((4-methoxy-3,5-bis(methylcarbamoyl)benzyl)amino)-2-oxoethyl)-1,4,7,10-tetraazacyclododecane-1,4,7-tricarboxylate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
5-(aminomethyl)-2-methoxy-N1,N3-dimethylisophthalamide;
With
N-ethyl-N,N-diisopropylamine;
In
N,N-dimethyl-formamide;
at 0 ℃;
for 0.25h;
2-(4,7,10-tris(tert-butoxycarbonyl)-1,4,7,10-tetraazacyclododecan-1-yl)acetic acid;
With
HATU;
In
N,N-dimethyl-formamide;
at 0 - 22 ℃;
for 40h;
DOI:10.1021/ic500282n
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: methanol / 18 h / 65 °C
2.1: selenium(IV) oxide; naphthalene / 2.5 h / 85 - 215 °C / Inert atmosphere
3.1: hydroxylamine hydrochloride; pyridine / 24 h / 22 °C
4.1: hydrogenchloride; hydrogen; palladium 10% on activated carbon / ethanol; water / 16 h / 3750.38 Torr
5.1: triethylamine; silica gel / dichloromethane
6.1: N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 0.25 h / 0 °C
6.2: 40 h / 0 - 22 °C
With
pyridine; hydrogenchloride; selenium(IV) oxide; naphthalene; palladium 10% on activated carbon; hydroxylamine hydrochloride; hydrogen; silica gel; triethylamine; N-ethyl-N,N-diisopropylamine;
In
methanol; ethanol; dichloromethane; water; N,N-dimethyl-formamide;
2.1: |Riley Selenium Dioxide Oxidation;
DOI:10.1021/ic500282n
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: potassium carbonate / acetone / 16 h / 56 °C
2.1: methanol / 18 h / 65 °C
3.1: selenium(IV) oxide; naphthalene / 2.5 h / 85 - 215 °C / Inert atmosphere
4.1: hydroxylamine hydrochloride; pyridine / 24 h / 22 °C
5.1: hydrogenchloride; hydrogen; palladium 10% on activated carbon / ethanol; water / 16 h / 3750.38 Torr
6.1: triethylamine; silica gel / dichloromethane
7.1: N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 0.25 h / 0 °C
7.2: 40 h / 0 - 22 °C
With
pyridine; hydrogenchloride; selenium(IV) oxide; naphthalene; palladium 10% on activated carbon; hydroxylamine hydrochloride; hydrogen; silica gel; potassium carbonate; triethylamine; N-ethyl-N,N-diisopropylamine;
In
methanol; ethanol; dichloromethane; water; N,N-dimethyl-formamide; acetone;
3.1: |Riley Selenium Dioxide Oxidation;
DOI:10.1021/ic500282n
