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发明公开
CN108117554A 一种球磨法制备伊曲茶碱晶型Ⅲ的方法 无效 - 撤回

  • 专利标题： 一种球磨法制备伊曲茶碱晶型Ⅲ的方法
  • 专利标题（英）： Method of preparing istradefylline crystal form III by means of ball-milling method
  • 申请号： CN201810190550.2
    申请日： 2018-03-08
  • 公开(公告)号： CN108117554A
    公开(公告)日： 2018-06-05
  • 发明人: 董丹丹
  • 申请人： 董丹丹
  • 申请人地址： 贵州省安顺市普定县城关镇红旗路晨光雅苑3#2-102
  • 专利权人： 董丹丹
  • 当前专利权人： 董丹丹
  • 当前专利权人地址： 贵州省安顺市普定县城关镇红旗路晨光雅苑3#2-102
  • 主分类号： C07D473/06
  • IPC分类号： C07D473/06
一种球磨法制备伊曲茶碱晶型Ⅲ的方法
摘要：
本发明公开了一种球磨法制备伊曲茶碱晶型Ⅲ的方法，将伊曲茶碱置于球磨罐中，按照每100mg伊曲茶碱加入到15～20uL的四氢呋喃中，以5～10HZ的研磨频率研磨60～100min，制得伊曲茶碱晶型Ⅲ；本发明制备工艺新颖，提高了反应收率，最终制得的伊曲茶碱产物纯度经检测达到99.6%，该方法制得的伊曲茶碱作为原料经特定溶剂、研磨频率与研磨时间的配合，制备得到的伊曲茶碱晶型Ⅲ光学纯度在99.9%以上，大大提高了产品的质量。
摘要（英）：

The invention discloses a method of preparing an istradefylline crystal form III by means of a ball-milling method. The method comprises the following steps: putting istradefylline in a ball-milling tank; adding 100mg of istradefylline into 15-20 mu L tetrahydrofuran; and grinding the mixture at a grinding frequency of 5-10HZ for 60-100min to obtain the tetrahydrofuran crystal form III. The preparation method is novel in process, the reaction yield is improved, and the purity of the finally prepared istradefylline product reaches 99.6% through detection. The istradefylline prepared by the method is matched with a special solvent, and the grinding frequency and the grinding time as a raw material, so that the optical purity of the prepared istradefylline crystal form III is 99.9% or above,and the product quality is improved greatly.

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