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Water → 5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide

HRID 1468287
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1468287
[Cl:1][C:2]1[N:7]2[C:8]([CH2:15][CH:16]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18][CH2:17]3)=[C:9]([C:11]([F:14])([F:13])[F:12])[N:10]=[C:6]2[CH:5]=[C:4]([C:24]([OH:26])=O)[CH:3]=1.CCN=C=NCCCN(C)C.Cl.[CH:39]1[CH:40]=[CH:41][C:42]2N(O)N=[N:45][C:43]=2[CH:44]=1.O.NC1C=CC=CC=1>CN(C=O)C>[Cl:1][C:2]1[N:7]2[C:8]([CH2:15][CH:16]3[CH2:21][CH2:20][C:19]([F:22])([F:23])[CH2:18][CH2:17]3)=[C:9]([C:11]([F:14])([F:12])[F:13])[N:10]=[C:6]2[CH:5]=[C:4]([C:24]([NH:45][C:43]2[CH:44]=[CH:39][CH:40]=[CH:41][CH:42]=2)=[O:26])[CH:3]=1
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Komponenten

7

Edukt 5

HCID 962WaterHCID 6115AnilineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 867100955-Chloro-3-(4,4-difluorocyclohexylmethyl)-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxylic acid

Produkt 1

HCID 86710096
5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide
Ausbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A part of the crude product of 5-chloro-3-(4,4-difluorocyclohexylmethyl)-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxylic acid obtained in step 3 (28 mg) was dissolved in DMF (2.0 mL), and the solution was stirred overnight at room temperature after adding EDC.HCl (27 mg, 0.141 mmol), HOBt.H2O (22 mg, 0.141 mmol), and aniline (13 mg, 0.141 mmol). The reaction mixture was extracted with ethyl acetate after adding a sodium hydrogen carbonate aqueous solution. The organic layer was washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was then evaporated under reduced pressure. The residue was purified by preparative thin-layer chromatography (chloroform/methanol=9/1) to give 5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide (18.0 mg, two-step yield 62%).

Aufarbeitung

  1. extractionThe reaction mixture was extracted with ethyl acetate
  2. additionafter adding a sodium hydrogen carbonate aqueous solution
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was then evaporated under reduced pressure
  6. customThe residue was purified by preparative thin-layer chromatography (chloroform/methanol=9/1)

Quellen und Nachweise

ORD-Eintrag
ord-039b3402046346d294fd5588e9060bea
Quelldatensatz
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09000186B2

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