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Water → Methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinate

HRID 69926
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 69926
[NH2:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1.[F:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[C:15]=1B(O)O.O.CCOC(C)=O>COCCOC.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[NH2:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[N:4][C:5]([C:15]2[C:14]([F:13])=[CH:19][CH:18]=[CH:17][C:16]=2[F:20])=[C:6]([F:8])[CH:7]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 27343362,6-Difluorophenylboronic acid2×HCID 66652559Methyl 3-amino-5-fluoropicolinate

Produkt 1

HCID 59226608Methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418807
HCID 178418807, Verbindung
Katalysator
HCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

To a solution of methyl 3-amino-5-fluoropicolinate (1.0 equiv.) in DME/2M Na2CO3 (3:1, 0.05 M) equipped with microwave vial was added 2,6-difluorophenylboronic acid (3.0 equiv.) and Pd(dppf)Cl2-DCM (0.1 equiv.). The reaction mixture was heated to 140° C. for 10 min in microwave reactor. After 2,6-difluorophenylboronic acid (3.0 equiv.) was added more, the reaction mixture was heated once more to 140° C. for 10 min in microwave reactor. After the reaction mixture was cooled to room temperature, H2O and EtOAc were added and the organic phase was washed with brine, then dried with Na2SO4, and concentrated. The crude material was purified via preparative HPLC. The pure methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinate was obtained after the pure fractions were neutralized with NaHCO3, extracted with EtOAc, and concentrated (34%). The methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinate (1.0 equiv.) was dissolved in THF and MeOH (2:1, 0.2 M) followed by addition of LiOH (1.8 equiv., 1 M aqueous solution). After the reaction mixture was stirred for 1.5 h at room temperature, the reaction mixture was quenched with 1 N HCl solution (1.8 equiv.) and extracted with EtOAc. The organic phase was washed with brine, then dried with Na2SO4, and concentrated. The crude 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinic acid was used for the next step without further purification (88%). LCMS (m/z): 269.0 (MH+); LC Rt=3.26 min.

Aufarbeitung

  1. temperaturethe reaction mixture was heated once more to 140° C. for 10 min in microwave reactor
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. washthe organic phase was washed with brine
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated
  6. customThe crude material was purified via preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-4fcc44cecb0a434788623170b849d73c
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08822497B2

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