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Dimethylformamide → 3-(3-Isopentylthio-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane fumarate

HRID 726979
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 726979
Cl[C:2]1[C:6]([CH:7]2[CH:12]3[CH2:13][CH2:14][N:9]([CH2:10][CH2:11]3)[CH2:8]2)=[N:5][S:4][N:3]=1.[OH2:15].[SH2:16].[Na].[C:18](=[O:21])([O-:20])[O-].[K+].[K+].Br[CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28].CN([CH:33]=[O:34])C>O>[C:33]([OH:34])(=[O:15])/[CH:13]=[CH:14]/[C:18]([OH:20])=[O:21].[CH2:25]([S:16][C:2]1[C:6]([CH:7]2[CH:12]3[CH2:13][CH2:14][N:9]([CH2:10][CH2:11]3)[CH2:8]2)=[N:5][S:4][N:3]=1)[CH2:26][CH:27]([CH3:29])[CH3:28]
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Komponenten

7

Edukt 5

HCID 6228Dimethylformamide2×HCID 78911-Bromo-3-methylbutaneHCID 11430Potassium CarbonateHCID 99427073-Chloro-4-quinuclidin-3-yl-1,2,5-thiadiazole2×HCID 53442613Sodium hydrogen sulfide hydrate

Produkt 1

HCID 21708633
3-(3-Isopentylthio-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane fumarate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 3-(3-chloro-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane (Compound 8) (420 mg, 1.83 mmol), sodiumhydrogen sulfide monohydrate (245 mg, 3.70 mmol) and potassium carbonate (780 mg, 5.64 mmol) in DMF (20 ml) was stirred at room temperature for 2 h. A solution of 1-bromo-3-methylbutane (420 mg, 2.75 mmol) in DMF (5 ml) was added, and the reaction mixture was stirred at room temperature for 3 h. Water (20 ml) was added and the mixture was extracted with ethyl acetate (3×100 ml). The combined extract was washed with brine, dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (eluent: CH2Cl2 :MeOH:NH4OH (8:2:0.5%)) to give the free base of the desired product in 400 mg yield. Crystallization of the residue with fumaric acid from isopropanol/ether gave the title compound in 370 mg yield. (Compound 99). M.p. 130°-132° C.

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate (3×100 ml)
  2. extractionThe combined extract
  3. washwas washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography (eluent: CH2Cl2 :MeOH:NH4OH (8:2:0.5%))

Quellen und Nachweise

ORD-Eintrag
ord-472cfd365f1d4322be8e4ea5c507ec48
Quelldatensatz
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05712271

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