tris(hydroxymethyl)-methylazanium

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

実験手順: 3.0 g (0.010 mol) of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide are suspended in 70 ml of methanol; 2.4 g of tris-(hydroxymethyl)-aminomethane are added and the whole is stirred at room temperature for 12 hours, during which time the free acid goes into solution and precipitates again in the form of a salt. The resulting precipitate is filtered off, washed with cold methanol and dried under greatly reduced pressure at 60°. The tris-(hydroxymethyl)-methylammonium salt of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide is obtained in the form of white crystals having a melting point of 203° (decomposition). precipitates again in the form of a salt The resulting precipitate is filtered off washed with cold methanol dried under greatly reduced pressure at 60°

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula II, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula II, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula III, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula III, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: 3.0 g (0.010 mol) of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide are suspended in 70 ml of methanol; 2.4 g of tris-(hydroxymethyl)-aminomethane are added and the whole is stirred at room temperature for 12 hours, during which time the free acid goes into solution and precipitates again in the form of a salt. The resulting precipitate is filtered off, washed with cold methanol and dried under greatly reduced pressure at 60°. The tris-(hydroxymethyl)-methylammonium salt of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide is obtained in the form of white crystals having a melting point of 203° (decomposition). precipitates again in the form of a salt The resulting precipitate is filtered off washed with cold methanol dried under greatly reduced pressure at 60°

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

実験手順: 3.0 g (0.010 mol) of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide are suspended in 70 ml of methanol; 2.4 g of tris-(hydroxymethyl)-aminomethane are added and the whole is stirred at room temperature for 12 hours, during which time the free acid goes into solution and precipitates again in the form of a salt. The resulting precipitate is filtered off, washed with cold methanol and dried under greatly reduced pressure at 60°. The tris-(hydroxymethyl)-methylammonium salt of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide is obtained in the form of white crystals having a melting point of 203° (decomposition). precipitates again in the form of a salt The resulting precipitate is filtered off washed with cold methanol dried under greatly reduced pressure at 60°

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula II, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: In another embodiment of the present invention, there is provided a process for preparing the organic amine salt of formula III, comprising: (a) reacting D-isoglutamyl-D-tryptophan in water with an organic amine in water wherein the organic amine is tert-butylamine or N-methylglucamine or tromethamine; and (b) concentrating the solution by co-evaporating with isopropanol; adding of acetone to cause the precipitate of the salt; recovering the precipitate thereof; and vacuum drying the product to obtain the organic ammonium salt of formula III wherein A is tert-butylammonium or tris(hydroxymethyl)methylammonium or methyl-(2,3,4,5,6-pentahydroxy-hexyl)-ammonium. In another embodiment of the present invention, there is provided a process and (b) concentrating the solution by co-evaporating with isopropanol adding of acetone recovering the precipitate and vacuum drying the product

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

実験手順: 3.0 g (0.010 mol) of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide are suspended in 70 ml of methanol; 2.4 g of tris-(hydroxymethyl)-aminomethane are added and the whole is stirred at room temperature for 12 hours, during which time the free acid goes into solution and precipitates again in the form of a salt. The resulting precipitate is filtered off, washed with cold methanol and dried under greatly reduced pressure at 60°. The tris-(hydroxymethyl)-methylammonium salt of 1,1',5,5'-tetrahydro-4-hydroxy-2,2'-dioxo-[3,4'-bi-2H-pyrrole]-1,1'-diacetic acid diamide is obtained in the form of white crystals having a melting point of 203° (decomposition). precipitates again in the form of a salt The resulting precipitate is filtered off washed with cold methanol dried under greatly reduced pressure at 60°