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Triphenylphosphine → HCID 69085829, Verbindung

HRID 2362465
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2362465
C(C1C=C([C@@H]2[C@@H:13]([C:14]3C=CC=C(F)C=3)[O:12]C(=O)N2)C=[N:7]C=1)#C.F[C:23]1[CH:28]=[CH:27][C:26]([F:29])=[CH:25][C:24]=1[C@H:30]1[O:34][C:33](=[O:35])[NH:32][C@@H:31]1[C:36]1[CH:37]=[N:38][CH:39]=[C:40]([C:42]#[CH:43])[CH:41]=1.FC1C=C(C=CC=1)C=O.Br[C:54]1[CH:59]=[N:58][CH:57]=[CH:56][N:55]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(C(C)C)CC)(C)C>[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cu]I.CN(C)C=O>[C:13]([O-:12])(=[O:34])[CH3:14].[NH4+:7].[F:29][C:26]1[CH:25]=[C:24]([C@H:30]2[O:34][C:33](=[O:35])[NH:32][C@@H:31]2[C:36]2[CH:37]=[N:38][CH:39]=[C:40]([C:42]#[C:43][C:54]3[CH:59]=[N:58][CH:57]=[CH:56][N:55]=3)[CH:41]=2)[CH:23]=[CH:28][CH:27]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 6

HCID 11776TriphenylphosphineHCID 680093-FluorobenzaldehydeHCID 81531DiisopropylethylamineHCID 6428002-BromopyrazineHCID 86673452HCID 86673452, VerbindungHCID 86673456HCID 86673456, Verbindung

Produkt 2

HCID 517165
Ammonium Acetate
HCID 69085829HCID 69085829, VerbindungAusbeute 48 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 6102075Dichlorobis(triphenylphosphine)palladiumKatalysatorHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

(4R,5R)-4-(5-ethynylpyridin-3-yl)-5-(3-fluorophenyl)oxazolidin-2-one (50 mg, 0.177 mmol; prepared in analogous fashion to the preparation of (4R,5R)-5-(2,5-difluorophenyl)-4-(5-ethynylpyridin-3-yl)oxazolidin-2-one starting from 3-fluorobenzaldehyde in place of 2,5-difluorobenzaldehyde), 2-bromopyrazine (31.0 mg, 0.195 mmol), bis(triphenylphosphine) palladium (II) chloride (6.22 mg, 8.86 mmol), triphenylphosphine (9.29 mg, 0.035 mmol), and copper (I) iodide (1.687 mg, 8.86 mmol) were combined in a microwave vial. Dimethylformamide (0.250 mL) and diisopropylethylamine (0.75 mL) were added resulting in a biphasic mixture. Nitrogen was bubbled through the vessel for 10 min, the vessel was capped and the reaction was run at 120° C. for 25 min on a Biotage microwave reactor. The diisopropylethylamine removed in vacuo, the remaining solution was diluted with methanol and the solution was purified via preparative liquid chromatography (Sunfire C18 19×100 mm 5 nm, A=95% H2O/5% Acetonitrile, B=95% Acetonitrile/5% H2O, Modifier 10 mM Ammonium Acetate, 0.00 min=20% B, 8.0 min=100% B, 13.0 min=100% B, Flow rate=25 mL/min) providing (4R,5R)-5-(3-fluorophenyl)-4-(5-(pyrazin-2-ylethynyl)pyridin-3-yl)oxazolidin-2-one (31 mg; 48%) as an amber foam. 1H NMR (500 MHz, CDCl3) δ ppm 8.89 (1H, br. s.), 8.81 (1H, s), 8.63 (1H, d, J=1.53 Hz), 8.57 (1H, d, J=2.44 Hz), 8.52 (1H, br. s.), 7.97 (1H, s), 7.41 (1H, td, J=7.93, 5.49 Hz), 6.94-7.19 (3H, m), 5.61 (1H, br. s.), 5.30 (1H, d, J=7.32 Hz), 4.81 (1H, d, J=7.32 Hz), Mass Spectral Anal. Calcd. for [M+H]+ C20H13FN4O2: 361.1. found 361.2.

Aufarbeitung

  1. customresulting in a biphasic mixture
  2. customNitrogen was bubbled through the vessel for 10 min
  3. customthe vessel was capped
  4. customThe diisopropylethylamine removed in vacuo
  5. additionthe remaining solution was diluted with methanol
  6. customthe solution was purified via preparative liquid chromatography (Sunfire

Quellen und Nachweise

ORD-Eintrag
ord-79c27586112c409a8d4cbbeed72848f5
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08691821B2

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