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7-Chloro-8-iodo-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridine → 7-Chloro-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridine-8-carbonitrile

HRID 1615899
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1615899
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]2[C:8]([CH2:11][C:12]([F:15])([F:14])[F:13])=[CH:9][N:10]=[C:4]2[C:3]=1I.[C:17]([Zn]C#N)#[N:18]>CN(C=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]2[C:8]([CH2:11][C:12]([F:15])([F:14])[F:13])=[CH:9][N:10]=[C:4]2[C:3]=1[C:17]#[N:18]
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Komponenten

5

Edukt 2

HCID 866964997-Chloro-8-iodo-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridineHCID 178514179HCID 178514179, Verbindung

Produkt 1

HCID 580811367-Chloro-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridine-8-carbonitrileAusbeute 142,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397HCID 178418397, VerbindungKatalysator
HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

A 2.0-5.0 mL microwave vial was charged with 7-chloro-8-iodo-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridine (30 mg, 0.083 mmol) dissolved in DMF (832 μl). To that stirring solution was added dicyanozinc (5.86 mg, 0.050 mmol) followed by tetrakis(triphenylphosphine)palladium(0) (28.8 mg, 0.025 mmol). The vial was sealed and degassed using sonication and ultra pure argon for 1 min. After which the vial was placed into a reaction block preheated to 120° C. After 5 hours, LCMS showed a good proportion of desired product by mass (m/z=260 [M+H]+Methanol/Water/Ammonium Acetate Phenomenex Luna C18, 30×2 mm, 3u ES+/−). The mixture was cooled to rt and diluted with sat'd sodium bicarbonate and EtOAc. The organic was washed with brine, dried with magnesium sulfate, concentrated under reduced pressure, and purified by flash chromatography: (4 g, equilibrated with none, loaded with DCM, initial waste: 0 mL, fraction size: 12 mL 16×100 mm, and eluted with EtOAc in hexanes 0% [20 mL], 0-100% [120 mL]). Collected fractions to give 7-chloro-3-(2,2,2-trifluoroethyl)imidazo[1,2-a]pyridine-8-carbonitrile (18.5 mg, 86% yield) as a plaque white solid. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 8.16 (d, J=7.3 Hz, 1H), 7.78 (s, 1H), 7.06 (d, J=7.3 Hz, 1H), 3.78 (q, J=9.8 Hz, 2H).

Aufarbeitung

  1. customThe vial was sealed
  2. customdegassed
  3. customsonication and ultra pure argon for 1 min
  4. custompreheated to 120° C
  5. additiondiluted with sat'd sodium bicarbonate and EtOAc
  6. washThe organic was washed with brine
  7. dry with materialdried with magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. custompurified by flash chromatography
  10. washinitial waste: 0 mL, fraction size: 12 mL 16×100 mm, and eluted with EtOAc in hexanes 0% [20 mL], 0-100% [120 mL])

Quellen und Nachweise

ORD-Eintrag
ord-b6a7e587f4f746b78c0cd60fb1a0c418
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08765767B2

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