294-90-6 | Cyclen

Introduction
Macrocyclic aza analogue of the crown ether 12-crown-4. Cyclen compounds are capable of selectively binding cations and are used as a ligand with chemicals used in MRI contrast (as well as other imaging) agents.

Specification of CAS: 294-90-6 Cyclen

Production of CAS: 294-90-6 Cyclen

Synthesis of Cyclen Intermediate

Put DMF1600kg, diethylenetriamine 100kg, diethanolamine 100.2kg, potassium carbonate 1382kg into the drying reactor, stir at 20-25℃ for 30min, start to add benzenesulfonyl chloride dropwise, 20-25℃, 3h after dripping 1070kg, heating to Stir the reaction at 30°C for 3h, continue heating to 110-115°C for 12h , recover DMF solvent to dryness under reduced pressure, add 2800kg of hot water to the reactor, stir for 2h at 80°C, filter while hot, and wash the filter cake with water To neutrality, dry to obtain 650 kg of off-white or light yellow solid intermediate with a yield of 91% (calculated by diethylene triamine).

Synthesis of Cyclen

650kg of intermediate and 3250kg of concentrated sulfuric acid were put into a dry reactor, heated to 90°C, reacted for 60h, after keeping warm, cooled to 20°C, started adding 3000kg of absolute ethanol dropwise, stirred and precipitated a large amount of off-white solid, after rinsing with a small amount of absolute ethanol , The filter cake is put into a reverse Chemicalbook reactor containing 2000kg of toluene, 30% liquid caustic soda is added dropwise to adjust until the pH of the feed liquid water layer is greater than or equal to 11, and after 30 minutes the pH is not changed, the solid is removed by filtration, and then the lower layer of water is removed. The phases were separated, the toluene feed liquid was concentrated to 1/4, frozen to -2°C, solid crystals were filtered out, and dried to obtain 104 kg of Lunhuan Tengning product with a yield of 73%.

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