Imatinib → Imatinib

HRID 1893735ノート

反応式

HRID 1893735 の反応式
C1([NH:7][S:8](=[O:11])(=[O:10])[OH:9])CCCCC1.[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([CH2:19][C:20]2[CH:48]=[CH:47][C:23]([C:24]([NH:26][C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[C:29]([NH:34][C:35]4[N:40]=[C:39]([C:41]5[CH:42]=[N:43][CH:44]=[CH:45][CH:46]=5)[CH:38]=[CH:37][N:36]=4)[CH:28]=3)=[O:25])=[CH:22][CH:21]=2)[CH2:15][CH2:14]1>C(O)C>[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([CH2:19][C:20]2[CH:21]=[CH:22][C:23]([C:24]([NH:26][C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[C:29]([NH:34][C:35]4[N:40]=[C:39]([C:41]5[CH:42]=[N:43][CH:44]=[CH:45][CH:46]=5)[CH:38]=[CH:37][N:36]=4)[CH:28]=3)=[O:25])=[CH:47][CH:48]=2)[CH2:15][CH2:14]1.[S:8](=[O:10])(=[O:9])([O-:11])[NH2:7]

参加物

5

反応物 2

HCID 5291ImatinibHCID 7533Cyclamate

生成物 2

HCID 5291ImatinibHCID 177700Sulfamate ion

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of N-cyclohexylsulphamic acid (Fluka, Buchs, Switzerland; 732 mg, 4 mmol) in ethanol (100 mL) is added to a solution of 4-[(4-methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]-benzamide (1.975 g, 4 mmol) in hot ethanol (150 mL at 90° C.). The solution is evaporated to dryness under reduced pressure and the resulting residue is re-crystallized from ethanol-isopropanol. The product is filtered-off and dried to afford 4-[(4-methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]-benzamide, sulphamate as a crystalline solid, having the following analytical properties: Analysis found: C, 61.13; H, 6.75; N, 15.87; O, 11.80; S, 4.57%. H2O, 1.69%. Calculated for C35H44N8O4S-0.40 i-PrOH-0.70 H2O: C, 61.28; H, 6.90; N, 15.79; O, 11.50; S, 4.52%. H2O, 1.78%.

後処理

  1. customThe solution is evaporated to dryness under reduced pressure
  2. customthe resulting residue is re-crystallized from ethanol-isopropanol
  3. customdried

出典と根拠

ORDレコード
ord-a2a8e569c67e4608adef6355672622de
出典データセット
uspto-grants-2013_08
特許番号
US08513256B2

反応ノート

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