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Cesium carbonate → 6-chloro-2-(5-fluoro-2-nitrophenylamino)-9-(tetrahydro-2H-pyran-4-yl)-7H-purin-8(9H)-one

HRID 2074151
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2074151
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7](=[O:17])[N:8]2[CH:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[C:4]([Cl:18])[N:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.Br[C:72]1[CH:77]=[C:76]([F:78])[CH:75]=[CH:74][C:73]=1[N+:79]([O-:81])=[O:80].CCN(C(C)C)C(C)C>C1(C)C=CC=CC=1.CC([O-])=O.CC([O-])=O.[Pd+2]>[Cl:18][C:4]1[N:3]=[C:2]([NH:1][C:72]2[CH:77]=[C:76]([F:78])[CH:75]=[CH:74][C:73]=2[N+:79]([O-:81])=[O:80])[N:10]=[C:9]2[C:5]=1[NH:6][C:7](=[O:17])[N:8]2[CH:11]1[CH2:12][CH2:13][O:14][CH2:15][CH2:16]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 10796Cesium carbonateHCID 81531DiisopropylethylamineHCID 634876Binap, (A+-)-HCID 27569932-Bromo-4-fluoro-1-nitrobenzeneHCID 576126442-amino-6-chloro-9-(tetrahydro-2H-pyran-4-yl)-7H-purin-8(9H)-one

Produkt 1

HCID 86622932
6-chloro-2-(5-fluoro-2-nitrophenylamino)-9-(tetrahydro-2H-pyran-4-yl)-7H-purin-8(9H)-one
Ausbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 167845palladium(II) acetateKatalysatorHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To an oven-dried vial was added 2-amino-6-chloro-9-(tetrahydro-2H-pyran-4-yl)-7H-purin-8(9H)-one (50 mg of HCl salt, 0.186 mmol, 1 equiv.) in anhydrous toluene (3 mL), then freshly grounded cesium carbonate (85 mg, 0.26 mmol, 1.4 equiv.) with stirring at room temperature under Ar. After 20 min, Pd(OAc)2 (12.5 mg, 0.019 mmol, 0.1 equiv.), racemic BINAP (17.3 mg, 0.028 mmol, 0.15 equiv.) and 1-bromo-5-fluoro-2-nitrobenzene (Oakwood) (53 mg, 0.24 mmol, 1.3 equiv.) were added as solids, followed by DIEA (50 μL, 1.5 equiv.). The vial was purged with Ar for 3 min, then closed and heated at 80° C. for 18 h. The reaction mixture was cooled to room temperature, diluted with 5% methanol in methylene chloride, filtered through a Nylon 0.45 μm filter, and the filter repeatedly washed with 5% methanol in methylene chloride. The filtrate was concentrated in vacuo and the resulting residue was purified using preparative TLC (silica gel, 4.25% methanol in methylene chloride) to give the desired product as a yellow solid (45.3 mg, 60% yield). 1H NMR (300 MHz, CDCl3) δ, ppm: 10.90 (s, 1H), 8.89 (dd, 1H), 8.45 (dd, 1H), 8.10 (br s, 1H), 6.92-6.83 (m, 1H), 4.75-4.60 (m, 1H), 4.28 (dd, 2H), 3.65 (app t, 2H), 2.82 (tdd, 2H), 1.90 (br d, 2H); MS (EI) m/z 409.1 (MH)+.

Aufarbeitung

  1. customThe vial was purged with Ar for 3 min
  2. customclosed
  3. temperatureThe reaction mixture was cooled to room temperature
  4. additiondiluted with 5% methanol in methylene chloride
  5. filtrationfiltered through a Nylon 0.45 μm
  6. filtrationfilter
  7. filtrationthe filter repeatedly
  8. washwashed with 5% methanol in methylene chloride
  9. concentrationThe filtrate was concentrated in vacuo
  10. customthe resulting residue was purified

Quellen und Nachweise

ORD-Eintrag
ord-5164aed74cc14070b1d989508aeff27e
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07919490B2

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