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Benzophenone imine → 4-[(4-Acetylpiperazin-1-yl)methyl]-2-amino-3-fluoropyridine

HRID 1355532
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1355532
Cl[C:2]1[C:7]([F:8])=[C:6]([CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16](=[O:18])[CH3:17])[CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.CC([O-])(C)C.[Na+].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.C(=[NH:84])(C1C=CC=CC=1)C1C=CC=CC=1.Cl.C1COCC1>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:16]([N:13]1[CH2:14][CH2:15][N:10]([CH2:9][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH2:84])[C:7]=2[F:8])[CH2:11][CH2:12]1)(=[O:18])[CH3:17]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 136809Benzophenone imineHCID 634876Binap, (A+-)-HCID 18422008HCl tetrahydrofuranHCID 185069231-[4-(2-Chloro-3-fluoro-pyridin-4-ylmethyl)-piperazin-1-yl]-ethanoneHCID 23676156Sodium t-butoxide

Produkt 1

HCID 18506814
4-[(4-Acetylpiperazin-1-yl)methyl]-2-amino-3-fluoropyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 4-[(4-acetylpiperazin-1-yl)methyl]-2-chloro-3-fluoropyridine (14-3, 85 mg, 0.31 mmole) in dry toluene (2 mL) was added NaOtBu (42 mg, 0.44 mmole), racemic BINAP (29 mg, 0.05 mmole), Pd2(dba)3 (14 mg, 0.02 mmole), and benzophenone imine (0.06 mL, 0.38 mmole) then the mixture was heated to 80° C. After 18 hr the mixture was cooled to RT. A solution of 1N HCl:THF (1:1, 10 mL) was added and the mixture stirred for 1 hr. The mixture was washed with EtOAc (2×). The aqueous layer was made basic with saturated NaHCO3 then extracted with EtOAc (3×). The combined organic layers were dried (Na2SO4), filtered, and concentrated. Flash column chromatography (gradient, 0-5% MeOH/CH2Cl2) gave the titled compound as a light yellow solid: 1H-NMR (500 MHz, CDCl3) δ 7.81 (d, 1 H, J=5.12 Hz), 6.71 (t, 1 H, J=4.88 Hz), 4.56 (bs, 2 H), 3.63 (t, 2 H, J=5.13 Hz), 3.56 (s, 2 H), 3.10 (t, 2 H, J=5.13 Hz), 2.46 (m, 2 H), 2.08 (s, 3 H); MS (ES) (M+H)+ 253.

Aufarbeitung

  1. temperatureAfter 18 hr the mixture was cooled to RT
  2. washThe mixture was washed with EtOAc (2×)
  3. extractionthen extracted with EtOAc (3×)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-b388004f05be4e1b84ef12675ddb6ff9
Quelldatensatz
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06586424B2

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