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N-methyl-2-pyrrolidone → HCID 178437679, Verbindung

HRID 869269
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 869269
Cl[C:2]1[C:3]([C:11]([NH2:13])=[O:12])=[N:4][C:5]([CH2:9][CH3:10])=[C:6](Cl)[N:7]=1.[Cl:14][C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][C:21]=1[S:22]([CH3:25])(=[O:24])=[O:23])[NH2:18].CN1C(=O)CCC1.[NH2:33][C@H:34]1[CH2:39][CH2:38][C@H:37]([OH:40])[CH2:36][CH2:35]1>C(OCC)(=O)C.C(O)C>[Cl:14][C:15]1[CH:16]=[C:17]([NH:18][C:2]2[C:3]([C:11]([NH2:13])=[O:12])=[N:4][C:5]([CH2:9][CH3:10])=[C:6]([NH:33][C@H:34]3[CH2:39][CH2:38][C@H:37]([OH:40])[CH2:36][CH2:35]3)[N:7]=2)[CH:19]=[CH:20][C:21]=1[S:22]([CH3:25])(=[O:24])=[O:23]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 13387N-methyl-2-pyrrolidoneHCID 108459213-Chloro-4-methanesulfonylanilineHCID 848199603,5-Dichloro-6-ethylpyrazine-2-carboxamideHCID 178511715HCID 178511715, Verbindung

Produkt 1

HCID 178437679HCID 178437679, VerbindungAusbeute 9,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
230 °C

Versuchsvorschrift

A mixture of 3,5-dichloro-6-ethylpyrazine-2-carboxamide (200 mg), 3-chloro-4-methylsulfonylaniline (374 mg) and NMP (1 mL) was stirred at 230° C. for 1 hour using a microwave reaction system. Thereafter, trans-4-aminocyclohexanol (524 mg) was added to the reaction liquid and stirred at 190° C. for 30 minutes using a microwave reaction system. After cooling, the reaction liquid was partitioned using ethyl acetate and water, and the organic layer was washed with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride. After drying over anhydrous magnesium sulfate, the solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:0 to 30:1) to give a crude product. This product was heated with ethanol and washed to give a light yellow solid. To the light yellow solid, ethyl acetate was added and heated, and insoluble materials were separated by filtration and the filtrate was concentrated. After the filtrate was concentrated, the residue was heated and washed with ethanol to give 3-{[3-chloro-4-(methylsulfonyl)phenyl]amino}-6-ethyl-5-[(trans-4-hydroxycyclohexyl)amino]pyrazine-2-carboxamide (39 mg) as a light yellow solid.

Aufarbeitung

  1. customa microwave reaction system
  2. stirringstirred at 190° C. for 30 minutes
  3. customa microwave reaction system
  4. temperatureAfter cooling
  5. customthe reaction liquid
  6. customwas partitioned
  7. washthe organic layer was washed with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride
  8. dry with materialAfter drying over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off
  10. customthe residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:0 to 30:1)
  11. customto give a crude product
  12. washwashed
  13. customto give a light yellow solid
  14. temperatureheated
  15. custominsoluble materials were separated by filtration
  16. concentrationthe filtrate was concentrated
  17. concentrationAfter the filtrate was concentrated
  18. temperaturethe residue was heated
  19. washwashed with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-fface636fc744497a68fab8ccd0e5bbc
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08969336B2

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