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Dichloromethane → 2-Fluoro-6-hydroxy-4-{2-(methylamino)-6-[(3R)-3-methyl-4-morpholinyl]-4-pyrimidinyl}benzonitrile

HRID 2367543
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Reaktionsgleichung

Reaktionsgleichung von HRID 2367543
Br[C:2]1[CH:9]=[C:8]([OH:10])[C:5]([C:6]#[N:7])=[C:4]([F:11])[CH:3]=1.C([O-])(=O)C.[K+].C(Cl)Cl.Cl[C:21]1[CH:26]=[C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][C@H:28]2[CH3:33])[N:24]=[C:23]([NH:34][CH3:35])[N:22]=1.C([O-])([O-])=O.[K+].[K+]>C(OCC)(=O)C.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].O1CCOCC1>[F:11][C:4]1[CH:3]=[C:2]([C:21]2[CH:26]=[C:25]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][C@H:28]3[CH3:33])[N:24]=[C:23]([NH:34][CH3:35])[N:22]=2)[CH:9]=[C:8]([OH:10])[C:5]=1[C:6]#[N:7]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 6344Dichloromethane2×HCID 11430Potassium CarbonateHCID 517044Potassium AcetateHCID 585046304-Bromo-2-fluoro-6-hydroxybenzonitrileHCID 585047304-Chloro-N-methyl-6-[(3R)-3-methyl-4-morpholinyl]-2-pyrimidinamine

Produkt 1

HCID 58504817
2-Fluoro-6-hydroxy-4-{2-(methylamino)-6-[(3R)-3-methyl-4-morpholinyl]-4-pyrimidinyl}benzonitrile
Ausbeute 93,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)Katalysator2×HCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a 20-mL screw-cap vial was added 4-bromo-2-fluoro-6-hydroxybenzonitrile (500 mg, 2.315 mmol), bis-pinacolato diboron (705 mg, 2.78 mmol), potassium acetate (568 mg, 5.79 mmol), PdCl2(dppf).CH2Cl2 adduct (95 mg, 0.116 mmol), and 1,4-dioxane (8 mL). The vial was capped and stirred for 4 h at 100° C. on a stirrer hot-plate. The reaction mixture was allowed to cool, then was diluted with ethyl acetate (50 mL) and washed with water (20 mL). The organic layer was dried over Na2SO4 and concentrated. The residue was added to a 20 mL microwave vial and 4-chloro-N-methyl-6-[(3R)-3-methyl-4-morpholinyl]-2-pyrimidinamine (0.279 g, 1.15 mmol), PdCl2(dppf).CH2Cl2 adduct (0.047 g, 0.058 mmol), K2CO3 (2 M, 1.725 mL, 3.45 mmol), and 1,4-dioxane (6 mL) were added. The resulting mixture was heated at 140° C. for 10 minutes in a microwave reactor. The organic layer was separated and the aqueous was diluted with water (10 mL), neutralized with 0.1 N HCl (pH paper), then extracted with EtOAc (3×50 mL). The organics were combined, and then dried over Na2SO4. The dried solution was concentrated, then purified by flash chromatography 0-10% CH3OH in CH2Cl2 (24 g column, dry-loaded) to afford the title compound (0.37 g) as a brown solid. LC-MS (ES) m/z=344 [M+H]+.

Aufarbeitung

  1. customTo a 20-mL screw-cap vial
  2. customThe vial was capped
  3. temperatureto cool
  4. washwashed with water (20 mL)
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated
  7. additionThe residue was added to a 20 mL microwave vial
  8. temperatureThe resulting mixture was heated at 140° C. for 10 minutes in a microwave reactor
  9. customThe organic layer was separated
  10. additionthe aqueous was diluted with water (10 mL)
  11. extractionextracted with EtOAc (3×50 mL)
  12. dry with materialdried over Na2SO4
  13. concentrationThe dried solution was concentrated
  14. custompurified by flash chromatography 0-10% CH3OH in CH2Cl2 (24 g column, dry-loaded)

Quellen und Nachweise

ORD-Eintrag
ord-f7c8f0566dc941d5b494455d1cf3cff2
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08697685B2

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