p-Toluenesulfonate → Sorafenib Tosylate

HRID 332936

反応式

HRID 332936 の反応式
[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([O-:4])(=[O:3])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([NH:22][C:23]2[CH:39]=[CH:38][C:26]([O:27][C:28]3[CH:33]=[CH:32][N:31]=[C:30]([C:34]([NH:36][CH3:37])=[O:35])[CH:29]=3)=[CH:25][CH:24]=2)=[O:21])=[CH:15][C:14]=1[C:40]([F:43])([F:42])[F:41]>CO>[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([OH:4])(=[O:3])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([NH:22][C:23]2[CH:39]=[CH:38][C:26]([O:27][C:28]3[CH:33]=[CH:32][N:31]=[C:30]([C:34]([NH:36][CH3:37])=[O:35])[CH:29]=3)=[CH:25][CH:24]=2)=[O:21])=[CH:15][C:14]=1[C:40]([F:43])([F:41])[F:42]

参加物

4

反応物 2

HCID 85570p-ToluenesulfonateHCID 216239Sorafenib

生成物 1

HCID 406563Sorafenib Tosylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.5 g of the tosylate salt of 4-{4-[({[4-chloro-3-(trifluoromethyl)phenyl]amino}carbonyl)-amino]phenoxy}-N-methylpyridine-2-carboxamide in the polymorph II are suspended in 15 ml of methanol and stirred at room temperature. After one week, the suspension is filtered and the residue dried at room temperature. Subsequently, the product is heat-treated at 150° C. for 30 min. The residue is analyzed by X-ray diffractometry and corresponds to the title compound in the polymorph III.

後処理

  1. waitAfter one week
  2. filtrationthe suspension is filtered
  3. customthe residue dried at room temperature
  4. additionSubsequently, the product is heat-treated at 150° C. for 30 min

出典と根拠

ORDレコード
ord-21e034fe98d94e6bb1f2b10d3807ccd0
出典データセット
uspto-grants-2014_11
特許番号
US08877933B2

関連ノート

読み込み中…