Nilotinib Hydrochloride Anhydrous → Nilotinib

HRID 72810

反応式

HRID 72810 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>CO.O>[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 1

HCID 16006490Nilotinib Hydrochloride Anhydrous

生成物 1

HCID 644241Nilotinib

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
65 °C

実験手順

4-Methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide hydrochloride (12 g) is suspended in 192 mL of methanol and 14.87 mL of water. The solution is heated to 64-66° C. in 10 minutes and kept for minutes at 66° C. The solution is then cooled down to 42° C. in 15 minutes and then seeded. The suspension is kept for 2.5 hours at 42° C. and cooled down to 20° C. in 7 hours and cooled down within 6 hours at −10° C. The suspension is kept for 79 hours before filtration under vacuum. The solid is washed 2 times with a cold mixture of methanol/water 66 mL/5.26 mL (−10° C.) and dried under vacuum at 70° C. for 20 hours to obtain form C 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. waitkept for minutes at 66° C
  2. temperatureThe solution is then cooled down to 42° C. in 15 minutes
  3. temperaturecooled down to 20° C. in 7 hours
  4. temperaturecooled down within 6 hours at −10° C
  5. filtrationThe suspension is kept for 79 hours before filtration under vacuum
  6. washThe solid is washed 2 times
  7. additionwith a cold mixture of methanol/water 66 mL/5.26 mL (−10° C.)
  8. customdried under vacuum at 70° C. for 20 hours

出典と根拠

ORDレコード
ord-ed72250b5751450cbb33c64155cadbd2
出典データセット
uspto-grants-2014_09
特許番号
US08829015B2

関連ノート

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