p-Toluenesulfonic acid → Sorafenib Tosylate

HRID 1749135

反応式

HRID 1749135 の反応式
[CH3:1][NH:2][C:3]([C:5]1[CH:6]=[C:7]([O:11][C:12]2[CH:13]=[CH:14][C:15]([NH:18][C:19]([NH:21][C:22]3[CH:23]=[CH:24][C:25]([Cl:32])=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:27]=3)=[O:20])=[CH:16][CH:17]=2)[CH:8]=[CH:9][N:10]=1)=[O:4].[C:33]1([CH3:43])[CH:38]=[CH:37][C:36]([S:39]([OH:42])(=[O:41])=[O:40])=[CH:35][CH:34]=1.CN(C)C=O>CO>[CH3:43][C:33]1[CH:38]=[CH:37][C:36]([S:39]([OH:42])(=[O:41])=[O:40])=[CH:35][CH:34]=1.[CH3:1][NH:2][C:3]([C:5]1[CH:6]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([NH:18][C:19]([NH:21][C:22]3[CH:23]=[CH:24][C:25]([Cl:32])=[C:26]([C:28]([F:31])([F:29])[F:30])[CH:27]=3)=[O:20])=[CH:14][CH:13]=2)[CH:8]=[CH:9][N:10]=1)=[O:4]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 216239Sorafenib

生成物 1

HCID 406563Sorafenib Tosylate収率 71.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

A mixture of sorafenib (5 gm), p-toluenesulfonic acid (3 gm), dimethylformamide (15 ml) and methanol (10 ml) were stirred for 20 minutes at room temperature. To the reaction mass was added methanol (80 ml) at 0 to 5° C. and stirred for 1 hour 30 minutes. The separated solid was filtered to obtain a wet solid. To the wet solid was added methanol (75 ml) and stirred for 2 hours at room temperature. The separated solid was filtered and then dried at 65 to 70° C. for 11 hours to obtain 4.9 gm of sorafenib tosylate polymorph III.

後処理

  1. stirringstirred for 1 hour 30 minutes
  2. filtrationThe separated solid was filtered
  3. customto obtain a wet solid
  4. stirringstirred for 2 hours at room temperature
  5. filtrationThe separated solid was filtered
  6. customdried at 65 to 70° C. for 11 hours

出典と根拠

ORDレコード
ord-0567bbdca21f42c3a5a62f104968d77c
出典データセット
uspto-grants-2015_10
特許番号
US09156789B2

関連ノート

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