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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-(4-(2-Aminopyridin-4-yloxy)-3-fluorophenyl)-2-fluoro-5-methylbenzamide

HRID 2373978
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Reaktionsgleichung

Reaktionsgleichung von HRID 2373978
[CH:1](N(C(C)C)CC)(C)C.N[C:11]1[N:16]=[CH:15][N:14]=[C:13]([O:17][C:18]2[CH:23]=[CH:22][C:21]([NH:24]C(NC(=O)CC3C=CC(F)=CC=3)=S)=[CH:20][C:19]=2[F:38])[CH:12]=1.[F:39][C:40]1[CH:48]=[CH:47][C:46]([CH3:49])=[CH:45][C:41]=1[C:42]([OH:44])=O.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[NH2:14][C:15]1[CH:1]=[C:13]([O:17][C:18]2[CH:23]=[CH:22][C:21]([NH:24][C:42](=[O:44])[C:41]3[CH:45]=[C:46]([CH3:49])[CH:47]=[CH:48][C:40]=3[F:39])=[CH:20][C:19]=2[F:38])[CH:12]=[CH:11][N:16]=1
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Komponenten

7

Edukt 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2428292-Fluoro-5-methylbenzoic acidHCID 115389121-(4-(6-Aminopyrimidin-4-yloxy)-3-fluorophenyl)-3-(2-(4-fluorophenyl)acetyl)thiourea2×

Produkt 1

HCID 59852870
N-(4-(2-Aminopyridin-4-yloxy)-3-fluorophenyl)-2-fluoro-5-methylbenzamide
Ausbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Diisopropylethylamine (0.035 mL, 0.200 mmol, 2.0 eq) was added to a solution of 4-(4-amino-2-fluorophenoxy)pyridin-2-amine (Compound B of Example 24, 0.022 g, 0.100 mmol, 1.0 eq), 2-fluoro-5-methyl benzoic acid (Aldrich, 0.015 g, 0.100 mmol, 1.0 eq), EDCI (0.021 g, 0.11 mmol, 1.1 eq) and HOBT (0.014 g, 0.100 mmol, 1.0 eq) in DMF (0.700 mL) at room temperature. The reaction mixture was stirred at room temperature for 8 h, quenched with saturated aqueous NaHCO3 solution and extracted with CHCl3 (3×10 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by reverse phase preparative HPLC (YMC ODS-A S10 30×500 mm, 30-90% aqueous MeOH with 0.1% TFA, 30 minute gradient) and the appropriate fractions were concentrated in vacuo. The concentrate was neutralized with saturated aqueous NaHCO3 solution and the mixture extracted with CHCl3 (3×30 mL). The combined organics were dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound (0.014 g, 40%) as a solid. 1H NMR (CD3OD) δ 7.67-7.80 (m, 2H), 7.36-7.45 (m, 3H), 7.03-7.14 (m, 2H), 6.14-6.16 (m, 1H), 5.89-5.90 (m, 1H), 2.29 (s, 3H); MS(ESI+) m/z 356 (M+H)+; HRMS(ESI+) calcd.: 356.1211, found: 356.1203.

Aufarbeitung

  1. customquenched with saturated aqueous NaHCO3 solution
  2. extractionextracted with CHCl3 (3×10 mL)
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by reverse phase preparative HPLC (YMC ODS-A S10 30×500 mm, 30-90% aqueous MeOH with 0.1% TFA, 30 minute gradient)
  7. concentrationthe appropriate fractions were concentrated in vacuo
  8. extractionthe mixture extracted with CHCl3 (3×30 mL)
  9. dry with materialThe combined organics were dried (Na2SO4)
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-eb8d0086df3d42e49a6b63cc6b11fda2
Quelldatensatz
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07459562B2

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