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Acetonitrile → Methyl 4-amino-5-fluoro-6-(4-formylphenyl)-3-vinylpicolinate

HRID 516561
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 516561
[F-].[K+].[NH2:3][C:4]1[C:9]([F:10])=[C:8](Cl)[N:7]=[C:6]([C:12]([O:14][CH3:15])=[O:13])[C:5]=1[CH:16]=[CH2:17].CC1(C)C(C)(C)OB([C:26]2[CH:33]=[CH:32][C:29]([CH:30]=[O:31])=[CH:28][CH:27]=2)O1.C(#N)C>C(Cl)Cl.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[NH2:3][C:4]1[C:9]([F:10])=[C:8]([C:26]2[CH:33]=[CH:32][C:29]([CH:30]=[O:31])=[CH:28][CH:27]=2)[N:7]=[C:6]([C:12]([O:14][CH3:15])=[O:13])[C:5]=1[CH:16]=[CH2:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 6342AcetonitrileHCID 522689Potassium FluorideHCID 27695364-Formylphenylboronic acid pinacol esterHCID 86668309Methyl 4-amino-6-chloro-5-fluoro-3-vinylpicolinate

Produkt 1

HCID 90408697Methyl 4-amino-5-fluoro-6-(4-formylphenyl)-3-vinylpicolinateAusbeute 97,5 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418476HCID 178418476, VerbindungKatalysator
HCID 962WaterLösungsmittel2×
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a 5-mL microwave safe vial was added potassium fluoride (0.378 g, 6.50 mmol), methyl 4-amino-6-chloro-5-fluoro-3-vinylpicolinate (0.5 g, 2.168 mmol), bis(triphenylphosphine)palladium(II) chloride (0.152 g, 0.217 mmol) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzaldehyde (0.528 g, 2.276 mmol). A mixture of water (1 mL) and acetonitrile (2 mL) was added and the reaction was capped and placed in a Biotage Initiator™ microwave reactor for 20 min at 115° C., with external IR-sensor temperature monitoring from the side of the vessel. Upon cooling to room temperature, the reaction mixture was diluted with CH2Cl2 (25 mL) and water (25 mL) and the organic layer was filtered through a cotton plug. An additional extraction using EtOAc (25 mL) was combined with the CH2Cl2 and dried over Na2SO4 (50 g). Following filtration of the combined organics through a cotton plug and concentration on a rotary evaporator, the residue was purified using a Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc to yield the title compound as a white solid (635 mg): 1H NMR (400 MHz, CDCl3) δ 10.08 (s, 1H), 8.13 (dd, J=8.3, 1.6 Hz, 2H), 8.03-7.93 (m, 2H), 6.91 (ddd, J=18.1, 11.6, 0.5 Hz, 1H), 5.73 (dd, J=11.5, 1.4 Hz, 1H), 5.60 (dd, J=18.1, 1.4 Hz, 1H), 4.77 (s, 2H), 3.94 (s, 3H); 19F NMR (376 MHz, CDCl3) δ −143.49; ESIMS m/z 301 ([M+H]+).

Aufarbeitung

  1. additionwas added
  2. customthe reaction was capped
  3. filtrationthe organic layer was filtered through a cotton plug
  4. extractionAn additional extraction
  5. dry with materialdried over Na2SO4 (50 g)
  6. filtrationfiltration of the
  7. concentrationcombined organics through a cotton plug and concentration
  8. customon a rotary evaporator
  9. customthe residue was purified
  10. customa Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc

Quellen und Nachweise

ORD-Eintrag
ord-d87fce373ac541c1976e08eed4adf297
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09113629B2

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