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Methanesulfonic Acid → 5-(5-Methoxybenzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)benzimidazole

HRID 74238
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 74238
Cl.[CH3:2][C:3]1[N:7]([CH:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[C:6]2[CH:14]=[CH:15][C:16]([C:18]([OH:20])=O)=[CH:17][C:5]=2[N:4]=1.N[C:22]1[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[CH:24][C:23]=1O.CC[N:33]=C=NCCCN(C)C.CS(O)(=O)=O.C(=O)([O-])O.[Na+]>O.CN(C=O)C>[CH3:29][O:28][C:27]1[CH:26]=[CH:25][C:24]2[O:20][C:18]([C:16]3[CH:15]=[CH:14][C:6]4[N:7]([CH:8]5[CH2:9][CH2:10][O:11][CH2:12][CH2:13]5)[C:3]([CH3:2])=[N:4][C:5]=4[CH:17]=3)=[N:33][C:23]=2[CH:22]=1
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Komponenten

8

Edukt 5

HCID 6395Methanesulfonic AcidHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 516892Sodium BicarbonateHCID 214926222-Amino-3-methoxyphenolHCID 674984452-methyl-1-(tetrahydropyran-4-yl)benzimidazole-5-carboxylic acid HCl salt

Produkt 1

HCID 67498170
5-(5-Methoxybenzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)benzimidazole
Ausbeute 3,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

2-methyl-1-(tetrahydropyran-4-yl)benzimidazole-5-carboxylic acid HCl salt (see Working Example 4-3) ((250 mg, 0.842 mmol), 2-amino-3-methoxyphenol (139 mg, 0.842 mmol), DMF (5 mL), and WSC (178 mg, 0.926 mmol) were stirred for 22 hours. Water was added and this was extracted with chloroform. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. To a dioxane (5 mL) solution of the solid obtained was added methanesulfonic acid (283 mg, 2.95 mmol), and this was heated to reflux for 18 hours. After the reaction solution was cooled, water and saturated aqueous sodium hydrogen carbonate solution were added, and this was extracted with chloroform. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The residue obtained was purified by silica gel column chromatography to yield the title compound (10 mg, 3.3% yield) as brown crystals.

Aufarbeitung

  1. extractionthis was extracted with chloroform
  2. customAfter the organic layer obtained
  3. dry with materialwas dried over anhydrous sodium sulfate, it
  4. filtrationwas filtered
  5. concentrationconcentrated
  6. customTo a dioxane (5 mL) solution of the solid obtained
  7. temperaturethis was heated
  8. temperatureto reflux for 18 hours
  9. temperatureAfter the reaction solution was cooled
  10. extractionthis was extracted with chloroform
  11. customAfter the organic layer obtained
  12. dry with materialwas dried over anhydrous sodium sulfate, it
  13. filtrationwas filtered
  14. concentrationconcentrated
  15. customThe residue obtained
  16. customwas purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-988f7cb6f5f746099d1c8f63c4fb5d31
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08829035B2

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