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Sodium Carbonate → 6-(2,6-dimethylphenyl)-N4-(4-{[2-(trifluoromethyl) pyridin-4-yl]oxy}phenyl)pyrimidine-2,4-diamine

HRID 729980
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 729980
Cl[C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=3)=[CH:12][CH:11]=2)[CH:3]=1.NC1N=C(Cl)C=C(Cl)N=1.FC(F)(F)C1C=C(OC2C=CC(N)=CC=2)C=CN=1.[CH3:54][C:55]1(B(O)O)[CH:60]=[CH:59][CH:58]=[C:57]([CH3:61])[CH2:56]1.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C>[CH3:54][C:55]1[CH:60]=[CH:59][CH:58]=[C:57]([CH3:61])[C:56]=1[C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=3)=[CH:12][CH:11]=2)[CH:3]=1
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Komponenten

7

Edukt 5

HCID 10340Sodium CarbonateHCID 655222-Amino-4,6-dichloropyrimidineHCID 578333536-chloro-N4-(4-{[2-(trifluoromethyl)pyridin-4-yl]oxy}phenyl)pyrimidine-2,4-diamineHCID 591345604-{[2-(Trifluoromethyl)pyridin-4-yl]oxy}anilineHCID 671059071,3-Dimethylphenylboronic acid

Produkt 1

HCID 11844998
6-(2,6-dimethylphenyl)-N4-(4-{[2-(trifluoromethyl) pyridin-4-yl]oxy}phenyl)pyrimidine-2,4-diamine
Ausbeute 56 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a mixture of 6-chloro-N4-(4-{[2-(trifluoromethyl)pyridin-4-yl]oxy}phenyl)pyrimidine-2,4-diamine (1.0 g, 2.6 mmol; available by condensation of 2-amino-4,6-dichloropyrimidine and {4-[(2-trifluromethylpyridin-4-yl)oxy]phenyl}amine, described in WO 2003/099771, which is hereby incorporated by reference) and 1,3-dimethylphenylboronic acid (786 mg, 5.2 mmol) in DMF (13 m]L) was added aqueous Na2CO3 (2 M, 3.9 mL) and tetrakis(triphenylphosphin)palladium (0) (303 mg, 0.26 mmol). The resulting mixture was degassed for 10 min before it was placed in a microwave reactor (Emrys optimizer by Personal Chemistry) at 150° C. for 20 min. The resulting mixture was cooled to rt before it was filtered and insoluble material was rinsed with DMF. The filtrate was concentrated under vacuo and dissolved in EtOAc. The resulting mixture was washed with water and the organic layer was dried over Na2SO4. Removal of the solvent under vacuo gave the crude material, which was purified with 40 M biotage eluting with Hex/EtOAc (1/1) to provide the title compound as an off-white solid (657 mg, 56%): 1H NMR (DMSO-d6): δ 9.27 (s, 1H), 8.59 (d, 1H), 7.86-7.90 (m, 2H), 7.35 (d, 1H), 7.04-7.17 (m, 6H), 6.35 (s, 2H), 5.86 (s, 1H), 2.10 (s, 6H) ppm; MS ES 452 (M+H)+, RT=2.76 min.

Aufarbeitung

  1. customThe resulting mixture was degassed for 10 min before it
  2. customwas placed in a microwave reactor
  3. filtrationwas filtered
  4. washinsoluble material was rinsed with DMF
  5. concentrationThe filtrate was concentrated under vacuo
  6. dissolutiondissolved in EtOAc
  7. washThe resulting mixture was washed with water
  8. dry with materialthe organic layer was dried over Na2SO4
  9. customRemoval of the solvent under vacuo
  10. customgave the crude material, which
  11. customwas purified with 40 M biotage
  12. washeluting with Hex/EtOAc (1/1)

Quellen und Nachweise

ORD-Eintrag
ord-0ee1fdee62e8485e8fb786199420e748
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07582646B2

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