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Sulfuric Acid → HCID 59136055, Verbindung

HRID 1960572
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1960572
CO[CH:3](OC)[CH:4]1[S:8][C:7]([C:9]2[NH:10][C:11]3[C:16]([CH:17]=2)=[CH:15][C:14]([O:18][CH2:19][CH2:20][O:21][CH3:22])=[CH:13][C:12]=3[N:23]([CH3:33])[S:24]([C:27]2[N:28]([CH3:32])[CH:29]=[CH:30][N:31]=2)(=[O:26])=[O:25])=[N:6][CH2:5]1.FC(F)(F)C(O)=O.S(=O)(=O)(O)O.Cl.[NH:49]1[CH2:54][CH2:53][S:52](=[O:55])[CH2:51][CH2:50]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>O1CCCC1.O.C(N(CC)CC)C>[CH3:22][O:21][CH2:20][CH2:19][O:18][C:14]1[CH:15]=[C:16]2[C:11](=[C:12]([N:23]([CH3:33])[S:24]([C:27]3[N:28]([CH3:32])[CH:29]=[CH:30][N:31]=3)(=[O:25])=[O:26])[CH:13]=1)[NH:10][C:9]([C:7]1[S:8][CH:4]([CH2:3][N:49]3[CH2:54][CH2:53][S:52](=[O:55])[CH2:51][CH2:50]3)[CH2:5][N:6]=1)=[CH:17]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 1118Sulfuric AcidHCID 6422Trifluoroacetic acidHCID 5049666Sodium triacetoxyborohydrideHCID 204414791Lambda4-thiomorpholin-1-one hydrochlorideHCID 59135952HCID 59135952, Verbindung

Produkt 1

HCID 59136055HCID 59136055, Verbindung
Ausbeute 18 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittelHCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a mixture of N-[2-[5-(dimethoxymethyl)-4,5-dihydro-1,3-thiazol-2-yl]-5-(2-methoxyethoxy)-1H-indol-7-yl]-N,1-dimethyl-1H-imidazole-2-sulfonamide (280 mg), trifluoroacetic acid (3.5 mL) and water (10.5 mL) was added concentrated sulfuric acid (3.5 mL), and the mixture was stirred at 60° C. for 3.5 hr. The excess trifluoroacetic acid was evaporated under reduced pressure, and the residue was neutralized with sodium hydrogencarbonate. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtrated, and the filtrate was concentrated under reduced pressure. The obtained crude product was dissolved in tetrahydrofuran (10 mL), thiomorpholine 1-oxide hydrochloride (103 mg) and triethylamine (0.1 mL) were added, and the mixture was stirred at room temperature for 15 min. Sodium triacetoxyborohydride (233 mg) was added, and the mixture was stirred at room temperature for 16 hr. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtrated, and the filtrate was concentrated under reduced pressure. The residue was silica gel column chromatography (methanol:ethyl acetate=0:100-10:90), and the obtained crude product was further purified by preparative HPLC to give the title compound (56 mg, yield 18%) as a white solid. MS: 581(MH+).

Aufarbeitung

  1. customThe excess trifluoroacetic acid was evaporated under reduced pressure
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltrated
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe obtained crude product
  8. stirringthe mixture was stirred at room temperature for 15 min
  9. stirringthe mixture was stirred at room temperature for 16 hr
  10. extractionthe mixture was extracted with ethyl acetate
  11. washThe organic layer was washed with saturated brine
  12. dry with materialdried over magnesium sulfate
  13. filtrationfiltrated
  14. concentrationthe filtrate was concentrated under reduced pressure
  15. customthe obtained crude product
  16. customwas further purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-caf17b7e9a8a4cb4800b94a67cb70c2c
Quelldatensatz
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08410087B2

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