2-Chloromandelic acid → Nilotinib 2-chloromandelate

HRID 1428269ノート

反応式

HRID 1428269 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:39])([F:38])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[Cl:40][C:41]1[CH:51]=[CH:50][CH:49]=[CH:48][C:42]=1[CH:43]([OH:47])[C:44]([OH:46])=[O:45]>C(OC)(C)(C)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:38])([F:39])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[Cl:40][C:41]1[CH:51]=[CH:50][CH:49]=[CH:48][C:42]=1[CH:43]([OH:47])[C:44]([O-:46])=[O:45]

参加物

4

反応物 2

HCID 977202-Chloromandelic acidHCID 644241Nilotinib

生成物 1

HCID 131732356Nilotinib 2-chloromandelate

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
5 °C

実験手順

Nilotinib base (0.300 g, 0.57 mmol) was dissolved in TFE (2 mL) at 40° C. to obtain a mixture. The mixture was stirred and added to a solution of 2-chloromandelic acid (0.106 g, 0.57 mmol) in TFE (1 mL) at 40° C. Stirring of the resulting clear solution was continued for about 4 h at 40° C. and the solution was subsequently cooled to 5° C. The mixture was kept at 5° C. overnight and then methyl tert-butyl ether (MTBE) (1.5 v/v) was added to the mixture at room temperature, leading to precipitation. The precipitate was filtered to give a white solid of Nilotinib 2-chloromandelate form I.

後処理

  1. customto obtain a mixture
  2. stirringStirring of the resulting clear solution
  3. waitThe mixture was kept at 5° C. overnight
  4. customleading to precipitation
  5. filtrationThe precipitate was filtered

出典と根拠

ORDレコード
ord-373eafd0bb2c429489afb73b8c33dde7
出典データセット
uspto-grants-2015_01
特許番号
US08937082B2

反応ノート

読み込み中…