2-(oxiran-2-ylmethyl)isoindole-1,3-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 50 g (144.3 mmol) of 1,4,7-tris(carboxymethyl)-1,4,7,10-tetraazacyclododecane (D03A) is dissolved in 250 ml of water, and the pH is set at 13 with 5N sodium hydroxide solution. Then, a solution of 38.12 g (187.6 mmol) of N(2,3-epoxypropyl)phthalimide (Aldrich) in 100 ml of dioxane is added in drops within one hour, stirred for 24 hours at 50° C., and the pH is kept at 13 by adding 5N sodium hydroxide solution. The solution is set at pH 2 with 10% hydrochloric acid and evaporated to the dry state in a vacuum. The residue is dissolved in some water and purified on an ion-exchange column (Reillex®=poly-(4-vinyl)pyridine (it is eluted with water). The main fractions are concentrated by evaporation in a vacuum, and final purification of the residue is achieved by chromatography on RP-18 (LiChroPrep®/mobile solvent: gradient that consists of tetrahydrofuran/methanol/water). After the main fractions are concentrated by evaporation, 63.57 g (71% of theory) of an amorphous solid is obtained. evaporated to the dry state in a vacuum The residue is dissolved in some water purified on an ion-exchange column (Reillex®=poly-(4-vinyl)pyridine (it is eluted with water) The main fractions are concentrated by evaporation in a vacuum final purification of the residue After the main fractions are concentrated by evaporation, 63.57 g (71% of theory) of an amorphous solid is obtained

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 50 g (144.3 mmol) of 1,4,7-tris(carboxymethyl)-1,4,7,10-tetraazacyclododecane (D03A) is dissolved in 250 ml of water, and the pH is set at 13 with 5N sodium hydroxide solution. Then, a solution of 38.12 g (187.6 mmol) of N(2,3-epoxypropyl)phthalimide (Aldrich) in 100 ml of dioxane is added in drops within one hour, stirred for 24 hours at 50° C., and the pH is kept at 13 by adding 5N sodium hydroxide solution. The solution is set at pH 2 with 10% hydrochloric acid and evaporated to the dry state in a vacuum. The residue is dissolved in some water and purified on an ion-exchange column (Reillex®=poly-(4-vinyl)pyridine (it is eluted with water). The main fractions are concentrated by evaporation in a vacuum, and final purification of the residue is achieved by chromatography on RP-18 (LiChroPrep®/mobile solvent: gradient that consists of tetrahydrofuran/methanol/water). After the main fractions are concentrated by evaporation, 63.57 g (71% of theory) of an amorphous solid is obtained. evaporated to the dry state in a vacuum The residue is dissolved in some water purified on an ion-exchange column (Reillex®=poly-(4-vinyl)pyridine (it is eluted with water) The main fractions are concentrated by evaporation in a vacuum final purification of the residue After the main fractions are concentrated by evaporation, 63.57 g (71% of theory) of an amorphous solid is obtained