Sorafenib → Sorafenib Tosylate

HRID 332935

反応式

HRID 332935 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:28]=[CH:27][C:15]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([NH:25][CH3:26])=[O:24])[CH:18]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][C:3]=1[C:29]([F:32])([F:31])[F:30].O.[C:34]1([CH3:44])[CH:39]=[CH:38][C:37]([S:40]([OH:43])(=[O:42])=[O:41])=[CH:36][CH:35]=1>C(O)C>[S:40]([C:37]1[CH:38]=[CH:39][C:34]([CH3:44])=[CH:35][CH:36]=1)([OH:43])(=[O:42])=[O:41].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:28]=[CH:27][C:15]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([NH:25][CH3:26])=[O:24])[CH:18]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][C:3]=1[C:29]([F:32])([F:30])[F:31]

参加物

4

反応物 2

HCID 216239SorafenibHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 406563Sorafenib Tosylate収率 91.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

903 g of 4-{4-[({[4-chloro-3-(trifluoromethyl)phenyl]amino}carbonyl)amino]phenoxy}-N-methyl-pyridine-2-carboxamide, prepared as described in WO 00/42012, are initially charged in 2700 ml of ethanol. 451.7 g of p-toluenesulfonic acid monohydrate are dissolved in 1340 g of ethanol and added dropwise at room temperature. The suspension is stirred at room temperature for 1 hour, then filtered off with suction, and the residue is washed three times with 830 ml each time of ethanol. The drying is effected at 50° C. under reduced pressure with supply of air. 1129.6 g of the title compound in the polymorph II are obtained.

後処理

  1. additionadded dropwise at room temperature
  2. filtrationfiltered off with suction
  3. washthe residue is washed three times with 830 ml each time of ethanol
  4. customis effected at 50° C. under reduced pressure

出典と根拠

ORDレコード
ord-c968c0b3de584495a5d0a7769e6e977e
出典データセット
uspto-grants-2014_11
特許番号
US08877933B2

関連ノート

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