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Cesium carbonate → 3-((3-Bromo-2-methylphenylamino)methyl)benzo[b]thiophene-2-carboxylic Acid

HRID 1918794
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1918794
Br[CH2:2][C:3]1[C:4]2[CH:15]=[CH:14][CH:13]=[CH:12][C:5]=2[S:6][C:7]=1[C:8]([O:10]C)=[O:9].[Br:16][C:17]1[C:18]([CH3:24])=[C:19]([CH:21]=[CH:22][CH:23]=1)[NH2:20].C(=O)([O-])[O-].[Cs+].[Cs+].O.[OH-].[Li+]>O.CO.C(#N)C>[Br:16][C:17]1[C:18]([CH3:24])=[C:19]([NH:20][CH2:2][C:3]2[C:4]3[CH:15]=[CH:14][CH:13]=[CH:12][C:5]=3[S:6][C:7]=2[C:8]([OH:10])=[O:9])[CH:21]=[CH:22][CH:23]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 10796Cesium carbonateHCID 1235383-Bromo-o-toluidineHCID 168937Lithium hydroxide, monohydrateHCID 21251535Methyl 3-(bromomethyl)-1-benzothiophene-2-carboxylate

Produkt 1

HCID 580441753-((3-Bromo-2-methylphenylamino)methyl)benzo[b]thiophene-2-carboxylic AcidAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer and reflux condenser was purged with nitrogen and charged with 103a (2.26 g, 7.92 mmol), 3-bromo-2-methylaniline (1.77 g, 9.51 mmol) and acetonitrile (50 mL). Cesium carbonate (7.75 g, 23.8 mmol) was added, and the mixture was stirred at 50° C. for 14 h. After this time, the reaction mixture was concentrated under reduced pressure and the resulting residue was dissolved in THF (15 mL), methanol (15 mL) and water (15 mL) and treated with lithium hydroxide monohydrate (1.30 g, 31.0 mmol). After stirring at room temperature for 14 h, the solvent was removed under reduced pressure and the resulting residue was acidified with 2 M hydrochloric acid to pH 5. The resulting mixture was extracted with ethyl acetate (3×30 mL), and the organic extracts were combined and dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by flash chromatography to afford 103b in 59% yield (1.70 g) as a white solid: mp 120-121° C.; 1H NMR (500 MHz, DMSO-d6) d 8.30 (d, 1H, J=12.5 Hz), 7.98 (d, 1H, J=12.5 Hz), 7.46 (m, 2H), 6.77 (m, 3H), 4.97 (s, 2H), 2.15 (s, 3H); MS (ESI+) m/z 378.9 (M+H).

Aufarbeitung

  1. customA 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer
  2. temperaturereflux condenser
  3. customwas purged with nitrogen
  4. concentrationAfter this time, the reaction mixture was concentrated under reduced pressure
  5. dissolutionthe resulting residue was dissolved in THF (15 mL)
  6. stirringAfter stirring at room temperature for 14 h
  7. customthe solvent was removed under reduced pressure
  8. extractionThe resulting mixture was extracted with ethyl acetate (3×30 mL)
  9. dry with materialdried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated under reduced pressure
  12. customThe resulting residue was purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-4de5064e8125489ba9f3222807ef86fb
Quelldatensatz
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08618107B2

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