Technology Process of 6,17-bis(benzyloxy)-1,6,12,17-tetraazacyclodocosane-2,5,13,16-tetrone
There total 19 articles about 6,17-bis(benzyloxy)-1,6,12,17-tetraazacyclodocosane-2,5,13,16-tetrone which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
In
dichloromethane;
at 20 ℃;
for 18h;
Inert atmosphere;
DOI:10.1002/ejoc.202000439
- Guidance literature:
-
Multi-step reaction with 7 steps
1: 1.) sodium iodide, 80percent sodium hydride / 1.) DMF, 15 min, 2.) DMF, 80 - 85 deg C, 4 h
2: 83 percent / conc. NH4OH, NH3 / Raney nickel / methanol / 3.5 h / 0 °C / 2844.3 - 2999.5 Torr
3: 65 percent / 4-dimethylaminopyridine, 1,3-dicyclohexylcarbodiimide / CH2Cl2 / 1.) 0 deg C, 45 min, 2.) room temp., 19 h
4: 83 percent / TFA / 0.33 h / Ambient temperature
5: 96 percent / pyridine / 1.5 h / 106 °C
6: 65 percent / conc. NH4OH, NH3 / Raney nickel / methanol / 3 h / 0 °C / 2844.3 - 2999.5 Torr
7: 43 percent / diphenylphosphoryl azide / dimethylformamide / 72 h / 0 - 5 °C
With
dmap; ammonium hydroxide; diphenylphosphoranyl azide; sodium hydride; dicyclohexyl-carbodiimide; trifluoroacetic acid; sodium iodide;
nickel;
In
pyridine; methanol; dichloromethane; N,N-dimethyl-formamide;
DOI:10.1016/S0040-4020(01)81074-7
- Guidance literature:
-
Multi-step reaction with 7 steps
1: 1.) sodium iodide, 80percent sodium hydride / 1.) DMF, 15 min, 2.) DMF, 80 - 85 deg C, 4 h
2: 83 percent / conc. NH4OH, NH3 / Raney nickel / methanol / 3.5 h / 0 °C / 2844.3 - 2999.5 Torr
3: 65 percent / 4-dimethylaminopyridine, 1,3-dicyclohexylcarbodiimide / CH2Cl2 / 1.) 0 deg C, 45 min, 2.) room temp., 19 h
4: 83 percent / TFA / 0.33 h / Ambient temperature
5: 96 percent / pyridine / 1.5 h / 106 °C
6: 65 percent / conc. NH4OH, NH3 / Raney nickel / methanol / 3 h / 0 °C / 2844.3 - 2999.5 Torr
7: 43 percent / diphenylphosphoryl azide / dimethylformamide / 72 h / 0 - 5 °C
With
dmap; ammonium hydroxide; diphenylphosphoranyl azide; sodium hydride; dicyclohexyl-carbodiimide; trifluoroacetic acid; sodium iodide;
nickel;
In
pyridine; methanol; dichloromethane; N,N-dimethyl-formamide;
DOI:10.1016/S0040-4020(01)81074-7
