-form of indicated salt comprises at least 90 wt.-% of crystals in -modification being crystals in -modification are non-hygroscopic that remains to be anhydrous practically into the glass climatic chamber at 25 C and relative humidity up to 93%. Preferably, crystalline -form comprises at least 95 wt.-% or 99 wt.-% of crystals in -modification that remains to be anhydrous at relative humidity 93% and at 25 C. Crystalline -form comprises usually at least 99 wt.-% of crystals in configuration with melting point below 225 C, preferably, melting point defining as onset of melting on thermogram obtained by differential scanning calorimetry, 217 C. Crystalline -form displays by the presence peak at refraction angle - equal to 2 obtained on roentgenogram by roentgen diffraction analysis being this peak shows relative intensity of lines equal to 65 as compared with the most intense line on roentgenogram. Usually, relative intensity of line in the following refraction angles 20 (relative intensity of lines are given as % in parentheses): 2 (40), 9,7 (26), 13,9 (23), 14,7 (57), 17,5 (90), 18,2 (65), 20,0 (76), 20,6 (100), 21,1 (89), 22,1 (38), 22,7 (44), 23,8 (23) and 29,8 (20) is 20% or more as compared with the most intense line on roentgenogram. Methods for preparing crystals in 30,8-modification involve decomposition of another crystalline form of acid-additive methanesulfonic acid salt and compound of the formula (I) using suitable polar solvent in suspension at temperature from 20 C to 50 C or dissolving another crystalline form or the parent amorphous product of methanesulfonic acid acid-additive salt and compound of the formula (I) in polar solvent at acceptable temperature in the range from 25 C to the dephlegmation point of reactive mass following by initiation of crystallization by addition of small amount of crystals in --modification as a seed at temperature from 20 C to 70 C. EFFECT: improved preparing method. 12 cl, 1 tbl, 3 dwg, 5 ex"/>
机译:酸加成甲烷-磺基磺酸盐和4-(4-甲基哌嗪-1-基-甲基)-N- [4-甲基-3-(4-吡啶--3-基)嘧啶-2-基亚胺基的结晶形式苯基]苯甲酰胺,其制备方法(变种)和药物成分
公开/公告号RU2208012C2
专利类型
公开/公告日2003-07-10
原文格式PDF
申请/专利权人 NOVARTIS AG (CH);
申请/专利号RU20000102914
申请日1998-07-16
分类号C07D401/04;A61K31/506;A61P35/00;C07D401/04;C07D239/00;C07D213/00;
国家 RU
入库时间 2022-08-21 23:43:46