TECHNOLOGY FOCUS - ORGANIC CHEMISTRY - Preparation (Claimed): Preparation of (I) comprises (1) taking N-1-(2-amino-ethyl)-ethane-1,2-diamine and then adding p-toluenesulfonyl chloride (126 g) in acetone solution (300 ml) and anhydrous potassium carbonate (91.2 g) in water (200 ml) and then dropping to diethylenetriamine (20.6 g or 0.20 mole) for 1.2-2 hours, reacting the mixture at room temperature for 4-4.5 hours, pouring the mixture into an ice water, adding water into the mixture for stirring, filtering the stirred mixture, and vacuum drying the filter cake with methanol to obtain (bis(2-(p-tolylsulfonyloxyamino)ethyl)amino)-4-methylbenzenesulfonate (II) as a white solid (103.2 g) and (91%), (2) taking 2-(2-hydroxy-ethylamino)-ethanol and then adding p-toluenesulfonyl chloride (126 g) in acetone solution (300 ml) and methylene dichloride solution, diethanolamine (21 g) and triethylamine (100 ml) in a reaction bottle and the dripping for 4-3 hours, reacting the mixture at room temperature for 4-4.5 hours, pouring the mixture into the ice water, separating the organic phase and then water washing for 3 times, drying the organic phase by anhydrous sodium sulfate and then filtering, evaporating the filtrate to obtain a yellow oily matter, and recrystallizing yellow oily matter with methanol and then vacuum drying to obtain (bis(2-(p-tolylsulfonylperoxy)ethyl)amino)-4-methylbenzenesulfonate (III) as white solid (99.1 g) and (88%), (3) adding (II) (34.4 g) and (III) (34 g) into dry N,N-dimethyl formamide (300 ml) and then reacting at 100-105 degrees C for 3-4 hours, cooling the mixture and then filtering and evaporating dimethyl fumarate until the solution is turbid, dropping methanol (150-60 ml), cooling and filtering the mixture, and washing the filter cake, washing by water for three times and then drying to obtain (4,7,10-tris(p-tolylsulfonyloxy)-1,4,7,10-tetrazacyclododec-1-yl) 4-methylbenzenesulfonate (IV) (30.1 g) and yield (63.7%), (4) adding (IV) into a sulfuric acid (60 ml) and then heating to dissolve at 110-115 degrees C for 48-50 hours, stirring the mixture, pouring the stirred mixture into absolute ethyl alcohol (200-250 ml) and the stirring for 0.5-1 hours, filtering the stirred mixture, adding filter cake into water (80-100 ml), decoloring the mixture using active carbon, adding concentrated hydrochloric acid (40-60 ml) to boil and then standing, filtering the mixture to obtain white solid, adding the white solid into water (30-50 ml), adjusting pH value of sodium hydroxide solution, adding chloroform and anhydrous sodium sulfate into the solid, and vaporizing the solvent for 3-5 times and then drying to obtain 1,4,7,10-tetraaza-cyclododecane as white solid (2.62 g) and yield (40%) (V), (5) adding (V) into triethylamine (4.5-9 g) and methylene dichloride (12-25 ml) or (145-255 ml) and then slowly dripping di-tert-butyl dicarbonate (17.70-35 g) at room temperature for less than 3 hours, stirring the mixture for 24-25 hours, decompressing and removing the solvent, and separating petroleum ether and ethyl acetate according to ratio of 1:1 by column chromatography to obtain tert-butyl acetate-ditert-butyl-1,4,7,10-tetrazacyclododecane-1,4-dicarboxylate (VI)as white solid (10.2-14.78 g) and yield (56.5-77.2%), (6) adding (VI) (10.68-15.84 g), potassium carbonate (7.64-9.84), potassium iodide (9.10-12.35 g) into reactor (500 ml), adding chloroacetonitrile (185-192 ml) and methyl cyanide (2.02-4.08 ml) into the mixture and then refluxing and reacting for 70-72 hours, removing the solvent, adding dichloromethane into the mixture and then filtering to remove inorganic salt, decompressing and removing the solvent, and separating petroleum ether and ethyl acetate according to ratio of 3:2 by column chromatography to obtain acetonitrile-tert-butyl acetate-ditert-butyl-1,4,7,10-tetrazacyclododecane-1,4-dicarboxylate (VII) as white solid (10.35-14.75 g) and yield (89.9%), (7) adding (VII) (7.12-10.20 g) and ammonia saturated ethanol solution (115-150 ml) into high pressure kettle (300 ml) and then uniformly mixing, adding Raney nickel (0.77-1.08 g) into the mixture, replacing air in the kettle and filling hydrogen at a pressure of 1.5-1.55 Mpa and then reacting at 24.5-26.5 degrees C for 48-50 hours, filtering the catalyst, and decompressing and removing the solvent and drying the mixture to obtain tert-butyl acetate-ditert-butyl 7-amino-1,4,7,10-tetrazacyclododecane-1,4-dicarboxylate (VIII) as a as white solid (6.5-8.3 g), where the product (VIII) has no need to separate, directly used for the next reaction, (8) adding (VIII) (3.3-6.9 g) and potassium carbonate (1.4-2.8 ml) into methyl cyanide (100-180 ml), stirring the mixture at 0-0.5 degrees C, dropping bromo-acetic acid phenyl ester (1.3-2.5 ml) and methyl cyanide (6-10 ml), finishing dripping, reacting the mixture at room temperature for 48-50 hours and then refluxing for 12 hours, decompressing and removing solvent, and separating ethyl acetate as eluent by column chromatography to obtain tert-butyl acetate-ditert-butyl 7-(2-((2-((Z,1E)-1-ethylidenebut-2-enoxy)-2-oxo-ethyl)amino)ethyl)-1,4,7,10-tetrazacyclododecane-1,4-dicarboxylate (IX) as colourless thick liquid (1.8-3.5 g) and yield (41.1-42.9%), (9) adding (IX) (3-5.5 g) and palladium on carbon (0.85-1.53 g) into the reaction bottle and then adding methanol (20-80 ml), reacting the mixture at a pressure of 1.5 Mpa and room temperature for 3-3.5 hours under hydrogen production, and filtering the mixture and removing the solvent to obtain 2-(2-(4,7-bis(tert-butoxycarbonyl)-1,4,7,10-tetrazacyclododec-1-yl)ethylamino)acetic acid-tert-butyl acetate (X) a white solid (2.1-4.168 g) and yield (81.2-84.7%), (10) adding (X) (58-290 mg), fullerene (72- 360 mg), poly-methylene unit (4.5-22.5 mg) into toluene (15-50 ml) and then reacting at 110-112 degrees C and then refluxing for 6-6.5 hours, decompressing and removing toluene, and separating petroleum ether and ethyl acetate according to ratio of 1:5 by fast column chromatography to obtain fullerene single macro-cycle polyamine intermediate of formula (XI) as a black solid (47-227.2 mg) and yield (31.6-37%), (11) adding (XI) (90-180 mg) in dichloromethane (50-80 ml), stirring the mixture under a condition of adding a trifluoroacetic acid (1-2 ml) at room temperature and then reacting for 18-24 hours, and monitoring the mixture by thin layer chromatography, and decompressing reaction mixture and removing the solvent and other low boiling-point impurities.