CRYSTALLINE D-ISOGLUTAMIL-D-TRIPTOPHANE AND D-ISOGLUTAMIL-D-TRIPTOPHANE MONOAMMONIUM SALT

摘要

1. Crystalline D-isoglutamyl-D-tryptophan, characterized by the X-ray powder diffraction pattern shown in FIG. 1. ! 2. Crystalline D-isoglutamyl-D-tryptophan, characterized by the following parameters of the powder X-ray diffraction pattern presented in the values of interplanar spacings d, Bragg angle 2θ and relative intensity (expressed as a percentage relative to the most intense line):! Angle, ° 2θ Value of d, E Relative intensity [%] 6.67 13.239 3 11.09 7.975 4.4 11.77 7.515 1.2 13.29 6.655 4 14.26 6.205 11.3 15.58 5.685 33, 3 16.81 5.269 28.9 17.27 5.13 30.4 18.35 4.832 12.2 18.87 4.7 95.8 20.05 4.424 63.6 20.9 4.247 33.2 22.03 4.032 17.1 22.88 3.884 10,023.74 3.744 97.9 24.54 3.625 41.9 25.44 3.499 20.3 25.69 3.465 12.1 26.31 3.384 16.4 27 3.3 27.4 27.75 3.212 24.9 28.18 3.164 19.3 28.79 3.099 6.8 29.13 3.063 6.2 29.91 2.985 79.2 31.04 2.879 8.6 31.49 2.839 33.7 32 , 54 2.749 4.4 33.29 2.689 9.3 33.97 2.637 10.5 34.99 2.562 17.3 35.54 2.524 21.8 36.14 2.483 5.136.74 2.444 5.9 37.35 2.406 7 7 38.31 2.348 25.6 39.01 2.307 20.3! 3. The method of obtaining in the aqueous phase of D-isoglutamyl-D-tryptophan, free of inorganic salts, comprising the following stages:! (a) obtaining a solution of the acid addition salt of H-D-iGlu-D-Trp-OH in an aqueous medium substantially free of an organic solvent; or obtaining a solution of the base addition salt of H-D-iGlu-D-Trp-OH in an aqueous medium substantially free of an organic solvent; ! (b) adjusting the pH to a value in the range of from about 2.0 to about 3.2 with an alkali metal hydroxide or inorganic acid solution to precipitate H-D-iGlu-D-Trp-OH; ! (c) recovering precipitated H-D-iGlu-D-Trp-OH; and! (d) vacuum drying the product obtained in step (c) to obtain H-D-iGlu-D-Trp-OH. ! 4. The crystalline ammonium salt H-D-iGlu-D-Trp-OH (1: 1), characterized by a powder x-ray, which