3-Cyano-5-(trifluoromethoxy)benzoic acid → 3-Cyano-N-{4-methyl-3-[6-(pyridin-3-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-5-(trifluoromethoxy)benzamide

HRID 1055730ノート

反応式

HRID 1055730 の反応式
[CH3:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[N:9]1[C:16]2[N:12]([N:13]=[C:14]([C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)[CH:15]=2)[CH:11]=[CH:10]1.[C:23]([C:25]1[CH:26]=[C:27]([CH:31]=[C:32]([O:34][C:35]([F:38])([F:37])[F:36])[CH:33]=1)[C:28](O)=[O:29])#[N:24]>>[C:23]([C:25]1[CH:26]=[C:27]([CH:31]=[C:32]([O:34][C:35]([F:36])([F:38])[F:37])[CH:33]=1)[C:28]([NH:6][C:5]1[CH:7]=[CH:8][C:2]([CH3:1])=[C:3]([N:9]2[C:16]3[N:12]([N:13]=[C:14]([C:17]4[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=4)[CH:15]=3)[CH:11]=[CH:10]2)[CH:4]=1)=[O:29])#[N:24]

参加物

3

反応物 2

HCID 219425323-Cyano-5-(trifluoromethoxy)benzoic acidHCID 897000234-Methyl-3-[6-(pyridin-3-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]aniline

生成物 1

HCID 896999143-Cyano-N-{4-methyl-3-[6-(pyridin-3-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-5-(trifluoromethoxy)benzamide

実験手順

Analogously to the procedure for Example 33, 50 mg (0.17 mmol) of the compound of Example 6A and 40 mg (0.18 mmol) of the compound of Example 41A were reacted with one another. After purification of the crude product by preparative HPLC, the product-containing fractions were concentrated to a small residual volume and made alkaline with a little saturated aqueous sodium bicarbonate solution. The precipitate formed was filtered off, washed with water and dried. This gave 56 mg (65% of theory) of the title compound.

後処理

  1. customAfter purification of the crude product by preparative HPLC
  2. concentrationthe product-containing fractions were concentrated to a small residual volume
  3. customThe precipitate formed
  4. filtrationwas filtered off
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-a39771ff0898428aa8d860ccf33c282c
出典データセット
uspto-grants-2016_07
特許番号
US09394309B2

反応ノート

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