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Methanol → N-Benzyl-4-methyl-2-(2-oxo-1,2-dihydropyridine-4-carboxamido)thiazole-5-carboxamide

HRID 45384
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 45384
[CH2:1]([NH:8][C:9]([C:11]1[S:15][C:14]([NH:16][C:17](=[O:26])[C:18]2[CH:23]=[CH:22][N:21]=[C:20]([O:24]C)[CH:19]=2)=[N:13][C:12]=1[CH3:27])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.I[Si](C)(C)C.CO>C(Cl)(Cl)Cl>[CH2:1]([NH:8][C:9]([C:11]1[S:15][C:14]([NH:16][C:17]([C:18]2[CH:23]=[CH:22][NH:21][C:20](=[O:24])[CH:19]=2)=[O:26])=[N:13][C:12]=1[CH3:27])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 887MethanolHCID 85247Trimethylsilyl iodideHCID 59369644N-Benzyl-2-(2-methoxyisonicotinamido)-4-methylthiazole-5-carboxamide

Produkt 1

HCID 59369671N-Benzyl-4-methyl-2-(2-oxo-1,2-dihydropyridine-4-carboxamido)thiazole-5-carboxamideAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212Chloroform
Lösungsmittel

Versuchsvorschrift

To a solution of N-benzyl-2-(2-methoxyisonicotinamido)-4-methylthiazole-5-carboxamide (0.26 g, 0.68 mmol) in anhydrous chloroform (15 mL) was added iodotrimethylsilane (1.37 g, 6.80 mmol) at 0° C. The mixture was refluxed for 16 hours and cooled down to ambient temperature. Methanol (3 mL) was added dropwise to quench the reaction. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate (100 mL) and washed with saturated sodium bicarbonate solution (2×100 mL), and brine (150 mL). The organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrate in vacuo. The residue was recrystallized from ethyl acetate and methanol to yield a colorless solid in 55% yield (0.13 g); m.p. 290-292° C.; 1H NMR (DMSO-d6, 300 MHz) δ 12.74 (s, br, 2H), 8.63 (t, J=5.9 Hz, 1H), 7.48 (d, J=6.8 Hz, 1H), 7.35-7.17 (m, 5H), 6.95 (d, J=1.6 Hz, 1H), 6.66 (dd, J=1.6, 6.8 Hz, 1H), 4.37 (d, J=5.9 Hz, 2H), 2.49 (s, 3H); 13C NMR (DMSO-d6, 75 MHz) δ 165.5, 162.6, 163.1, 162.0, 144.1, 140.0, 136.8, 128.7, 127.6, 127.1, 120.3, 119.2, 103.3, 43.0, 17.0; MS (ES+) m/z 369.2 (M+1).

Aufarbeitung

  1. temperatureThe mixture was refluxed for 16 hours
  2. customto quench
  3. customthe reaction
  4. customThe solvent was removed in vacuo
  5. dissolutionThe residue was dissolved in ethyl acetate (100 mL)
  6. washwashed with saturated sodium bicarbonate solution (2×100 mL), and brine (150 mL)
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationthe filtrate was concentrate in vacuo
  10. customThe residue was recrystallized from ethyl acetate and methanol
  11. customto yield a colorless solid in 55% yield (0.13 g)

Quellen und Nachweise

ORD-Eintrag
ord-d649733dfd09497fbb0652797e6c0d9a
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08541457B2

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