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Water → HCID 73775993, Verbindung

HRID 2207277
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2207277
[C:1]([C:3]1[CH:4]=[C:5]([S:23]([NH:26][C:27]2[S:28][CH:29]=[CH:30][N:31]=2)(=[O:25])=[O:24])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:11]=[N:12][C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:14][C:15]=1I)#[N:2].[F:32][C:33]1[C:38](B(O)O)=[CH:37][CH:36]=[CH:35][N:34]=1.C([O-])([O-])=O.[Na+].[Na+].O>CN(C)C=O.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>[C:1]([C:3]1[CH:4]=[C:5]([S:23]([NH:26][C:27]2[S:28][CH:29]=[CH:30][N:31]=2)(=[O:25])=[O:24])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:11]=[N:12][C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:14][C:15]=1[C:38]1[C:33]([F:32])=[N:34][CH:35]=[CH:36][CH:37]=1)#[N:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 27832702-Fluoropyridine-3-boronic acidHCID 90100535HCID 90100535, Verbindung

Produkt 1

HCID 73775993HCID 73775993, VerbindungAusbeute 30 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397
HCID 178418397, Verbindung
Katalysator
HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

10 mg (0.02 mmol) of 3-cyano-4-((4-iodo-6-phenylpyridin-3-yl)oxy)-N-(thiazol-2-yl)benzenesulfonamide was dissolved in 3 mL of N,N-dimethylformamide, and 3.7 mg (0.03 mmol) of (2-fluoropyridin-3-yl)boronic acid was added thereto, and then 2.0 mg (10 mol %) of Pd(PPh3)4, 5.6 mg (0.6 mmol) of Na2CO3, and 1 mL of H2O were added thereto. After reacting with microwave reactor at 120° C. for 5 minutes, the solvent was removed, and the remaining material was diluted with ethyl acetate and the organic layer was separated, and washed with saturated sodium chloride. The organic layer was collected, dried with magnesium sulfate to remove water, and concentrated under reduced pressure, and the residue was purified by column chromatography (developing solvent, hexane:ethyl acetate=3:1) to obtain 3 mg (30% yield) of the title compound.

Aufarbeitung

  1. customthe solvent was removed
  2. additionthe remaining material was diluted with ethyl acetate
  3. customthe organic layer was separated
  4. washwashed with saturated sodium chloride
  5. customThe organic layer was collected
  6. dry with materialdried with magnesium sulfate
  7. customto remove water
  8. concentrationconcentrated under reduced pressure
  9. customthe residue was purified by column chromatography (developing solvent, hexane:ethyl acetate=3:1)

Quellen und Nachweise

ORD-Eintrag
ord-013606f062c3405cb7f9500aad82430c
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09376429B2

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