(S)-4-AMINO-N-(1-(4-CHLOROPHENYL)-3-HYDROXYPROPYL)-1-(7H-PYRROLO[2,3-D]-PYRIMIDINE-4-YL)PIPERIDINE-4-CARBOXAMIDE IN CRYSTAL FORM

PROBLEM TO BE SOLVED: To acquire (S)-4-amino-N-(1-(4-chlorophenyl)-3-hydroxypropyl)-1-(7H-pyrrolo[2,3-d]-pyrimidine-4-yl)piperidine-4-carboxamide in a stable solid form, which is useful for remedy or prevention of a disease or a pathological state mediated by a protein kinase B(AKT).SOLUTION: Provided a method of preparing the compound of a crystal form B having a specific X-ray powder diffraction pattern and the crystal form. In the method, among crystal forms A, B and C of the compound, the compound of the form A or C is stirred in a slurry state in acetone or acetonitrile, in particular, in acetonitrile, and is converted into a form B, followed by filtering and drying. In the method, a duration may depend on a temperature of the slurry, and when the slurry is at 50°C, the compound reaches an allowable conversion yield when stirring for at least 3 days. Provided are pharmaceutical compositions containing these, and use of such a form in therapy.SELECTED DRAWING: Figure 3.2 【課題】プロテンキナーゼＢ（ＡＫＴ）により媒介される疾患又は病的状態の治療又は予防に有用である、安定な固体形態の（Ｓ）−４−アミノ−Ｎ−（１−（４−クロロフェニル）−３−ヒドロキシプロピル）−１−（７Ｈ−ピロロ［２，３−ｄ］−ピリミジン−４−イル）ピペリジン−４−カルボキサミドの取得。【解決手段】特定のＸ線粉末回折パターンを有する結晶形態Ｂの前記化合物，前記結晶形態を調製する方法。前記化合物の結晶形態Ａ，Ｂ，Ｃがあり、形態Ａ又はＣの前記化合物をアセトン又はアセトニトニル、特にアセトニトリル中にて、スラリー状態で撹拌して、形態Ｂへ変換させて、濾過及び乾燥させる方法。その期間は、スラリーの温度に依存する可能性があり、スラリーが５０℃であれば、前記化合物を少なくとも３日間撹拌すれば許容できる変換収率となる方法。それらを含む医薬組成物，および療法におけるそのような形態の使用。【選択図】図３．２