Water → Nilotinib

HRID 72809

反応式

HRID 72809 の反応式
Cl.[CH3:2][C:3]1[CH:27]=[CH:26][C:6]([C:7]([NH:9][C:10]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([N:20]3[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]3)[CH:11]=2)=[O:8])=[CH:5][C:4]=1[NH:28][C:29]1[N:34]=[C:33]([C:35]2[CH:36]=[N:37][CH:38]=[CH:39][CH:40]=2)[CH:32]=[CH:31][N:30]=1.O>CO>[CH3:2][C:3]1[CH:27]=[CH:26][C:6]([C:7]([NH:9][C:10]2[CH:15]=[C:14]([C:16]([F:17])([F:18])[F:19])[CH:13]=[C:12]([N:20]3[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]3)[CH:11]=2)=[O:8])=[CH:5][C:4]=1[NH:28][C:29]1[N:34]=[C:33]([C:35]2[CH:36]=[N:37][CH:38]=[CH:39][CH:40]=2)[CH:32]=[CH:31][N:30]=1

参加物

4

反応物 2

HCID 962WaterHCID 16006490Nilotinib Hydrochloride Anhydrous

生成物 1

HCID 644241Nilotinib

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

12 g 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide hydrochloride is dissolved in 192 mL of methanol and 21 ml of water at 52° C. The solution is heated to 64-66° C. in 10 minutes and let stand for 45 minutes. The solution is then cooled down in 3 hours at 0° C. The solution spontaneously crystallized before 0° C.; therefore, the cooling ramp was stopped at 20° C. and let stand with stirring for 2 days. The suspension is cooled down to 0° C. in 2 hours before filtration under vacuum to obtain form A of the hydrochloride salt of 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide.

後処理

  1. customat 52° C
  2. temperatureThe solution is then cooled down in 3 hours at 0° C
  3. customThe solution spontaneously crystallized before 0° C.
  4. customwas stopped at 20° C.
  5. temperatureThe suspension is cooled down to 0° C. in 2 hours before filtration under vacuum

出典と根拠

ORDレコード
ord-92fa8f28f2d24bde94debe8af8480d31
出典データセット
uspto-grants-2014_09
特許番号
US08829015B2

関連ノート

読み込み中…