3-tert-Butyl-N-(3-{6-[1-(4-methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methylphenyl)-5-(4-methylpiperazin-1-yl)benzamide → 3-tert-Butyl-5-(4-methylpiperazin-1-yl)-N-{4-methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]-pyrazol-1-yl]phenyl}benzamide

HRID 1055707ノート

反応式

HRID 1055707 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:40]=[C:41]([N:43]2[CH2:48][CH2:47][N:46]([CH3:49])[CH2:45][CH2:44]2)[CH:42]=1)[C:8]([NH:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]([N:18]2[C:25]3[N:21]([N:22]=[C:23]([C:26]4[CH:27]=[N:28][N:29](CC5C=CC(OC)=CC=5)[CH:30]=4)[CH:24]=3)[CH:20]=[CH:19]2)[CH:12]=1)=[O:9])([CH3:4])([CH3:3])[CH3:2]>FC(F)(F)C(O)=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:40]=[C:41]([N:43]2[CH2:48][CH2:47][N:46]([CH3:49])[CH2:45][CH2:44]2)[CH:42]=1)[C:8]([NH:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]([N:18]2[C:25]3[N:21]([N:22]=[C:23]([C:26]4[CH:27]=[N:28][NH:29][CH:30]=4)[CH:24]=3)[CH:20]=[CH:19]2)[CH:12]=1)=[O:9])([CH3:4])([CH3:2])[CH3:3]

参加物

3

反応物 1

HCID 896997983-tert-Butyl-N-(3-{6-[1-(4-methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methylphenyl)-5-(4-methylpiperazin-1-yl)benzamide

生成物 1

HCID 1366302363-tert-Butyl-5-(4-methylpiperazin-1-yl)-N-{4-methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]-pyrazol-1-yl]phenyl}benzamide

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
80 °C

実験手順

68 mg (76% pure, 79 μmol) of the compound of Example 57A were initially charged in 0.32 ml of trifluoroacetic acid and stirred at 80° C. for 3 h. The mixture was then purified directly by preparative HPLC (Method 29). The product fractions were concentrated under reduced pressure and the residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. This gave 41 mg (97% of theory) of the title compound.

後処理

  1. customThe mixture was then purified directly by preparative HPLC (Method 29)
  2. concentrationThe product fractions were concentrated under reduced pressure
  3. washwashed with saturated aqueous sodium bicarbonate solution
  4. dry with materialThe organic phase was dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-012239db16a44644a3e87568688e4e11
出典データセット
uspto-grants-2016_07
特許番号
US09394309B2

反応ノート

読み込み中…