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

HRID 1055709노트

반응식

HRID 1055709 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:39]=[C:40]([S:42]([F:47])([F:46])([F:45])([F:44])[F:43])[CH:41]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([N:16]2[C:23]3[N:19]([N:20]=[C:21]([C:24]4[CH:25]=[N:26][N:27](CC5C=CC(OC)=CC=5)[CH:28]=4)[CH:22]=3)[C:18]([CH3:38])=[CH:17]2)[CH:10]=1)=[O:7])#[N:2]>FC(F)(F)C(O)=O>[C:1]([C:3]1[CH:4]=[C:5]([CH:39]=[C:40]([S:42]([F:46])([F:44])([F:47])([F:43])[F:45])[CH:41]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([N:16]2[C:23]3[N:19]([N:20]=[C:21]([C:24]4[CH:28]=[N:27][NH:26][CH:25]=4)[CH:22]=3)[C:18]([CH3:38])=[CH:17]2)[CH:10]=1)=[O:7])#[N:2]

참가 물질

3

실험 절차

At 90° C., 115 mg (0.23 mmol) of the compound of Example 56A were stirred in 1.5 ml of trifluoroacetic acid for 60 min. The reaction was then concentrated under reduced pressure and the residue was purified by preparative HPLC (Method 21). The product fractions were combined, concentrated almost completely under reduced pressure and made alkaline with a little saturated aqueous sodium bicarbonate solution. The resulting precipitate was filtered off, washed with water and dried under high vacuum. This gave 60 mg (46% of theory) of the title compound.

후처리

  1. concentrationThe reaction was then concentrated under reduced pressure
  2. customthe residue was purified by preparative HPLC (Method 21)
  3. concentrationconcentrated almost completely under reduced pressure
  4. filtrationThe resulting precipitate was filtered off
  5. washwashed with water
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-5eec758e8fd74c1ebb6da8f08766f27a
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394309B2

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