N-(3-{6-[1-(4-Methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methyl-phenyl)-3-(4-methylpiperazin-1-yl)-5-(pentafluoro-lambda6-sulphanyl)benzamide → 3-(4-Methylpiperazin-1-yl)-N-{4-methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]-phenyl}-5-(pentafluoro-lambda6-sulphanyl)benzamide

HRID 1055703ノート

反応式

HRID 1055703 の反応式
COC1C=CC(C[N:8]2[CH:12]=[C:11]([C:13]3[CH:14]=[C:15]4[N:20]([C:21]5[CH:22]=[C:23]([NH:28][C:29](=[O:49])[C:30]6[CH:35]=[C:34]([S:36]([F:41])([F:40])([F:39])([F:38])[F:37])[CH:33]=[C:32]([N:42]7[CH2:47][CH2:46][N:45]([CH3:48])[CH2:44][CH2:43]7)[CH:31]=6)[CH:24]=[CH:25][C:26]=5[CH3:27])[CH:19]=[CH:18][N:16]4[N:17]=3)[CH:10]=[N:9]2)=CC=1>FC(F)(F)C(O)=O>[CH3:48][N:45]1[CH2:46][CH2:47][N:42]([C:32]2[CH:31]=[C:30]([CH:35]=[C:34]([S:36]([F:41])([F:38])([F:37])([F:39])[F:40])[CH:33]=2)[C:29]([NH:28][C:23]2[CH:24]=[CH:25][C:26]([CH3:27])=[C:21]([N:20]3[C:15]4[N:16]([N:17]=[C:13]([C:11]5[CH:10]=[N:9][NH:8][CH:12]=5)[CH:14]=4)[CH:18]=[CH:19]3)[CH:22]=2)=[O:49])[CH2:43][CH2:44]1

参加物

3

反応物 1

HCID 89699916N-(3-{6-[1-(4-Methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methyl-phenyl)-3-(4-methylpiperazin-1-yl)-5-(pentafluoro-lambda6-sulphanyl)benzamide

生成物 1

HCID 1366302453-(4-Methylpiperazin-1-yl)-N-{4-methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]-phenyl}-5-(pentafluoro-lambda6-sulphanyl)benzamide

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

At 80° C., 90 mg (0.12 mmol) of the compound of Example 48A were stirred in 0.61 ml of trifluoroacetic acid for 3 h. The reaction was then concentrated and the residue was purified by preparative HPLC (Method 18). The product fractions were concentrated, and the residue was dissolved in ethyl acetate and washed successively with saturated potassium carbonate solution and saturated sodium chloride solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. Drying of the residue under high vacuum gave 40 mg (53% of theory) of the title compound.

後処理

  1. concentrationThe reaction was then concentrated
  2. customthe residue was purified by preparative HPLC (Method 18)
  3. concentrationThe product fractions were concentrated
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washwashed successively with saturated potassium carbonate solution and saturated sodium chloride solution
  6. dry with materialThe organic phase was dried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customDrying of the residue under high vacuum

出典と根拠

ORDレコード
ord-e0d1b8d4bccd43ed93c9ced54555c752
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…