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2-Butanethiol → HCID 178456540, Verbindung

HRID 373231
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 373231
[Cl:1][C:2]1[C:3](=[O:50])[N:4]([CH2:47][CH2:48][CH3:49])[C:5](=[O:46])[N:6]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[N:26](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:7]=1Cl.[CH:51]([SH:55])([CH2:53][CH3:54])[CH3:52].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[C:3](=[O:50])[N:4]([CH2:47][CH2:48][CH3:49])[C:5](=[O:46])[N:6]([CH2:9][C:10]2[CH:11]=[CH:12][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:26][N:25]=[N:24][N:23]=3)=[CH:14][CH:15]=2)[C:7]=1[S:55][CH:51]([CH3:52])[CH2:53][CH3:54]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 105602-ButanethiolHCID 11430Potassium CarbonateHCID 19811540HCID 19811540, Verbindung

Produkt 1

HCID 178456540HCID 178456540, VerbindungAusbeute 56 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 5,6-dichloro-3-propyl-1-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione (0.22 g), sec-butylmercaptan (0.04 g) and potassium carbonate (0.09 g) in acetonitrile (5 ml) was heated under reflux for 4 hours. The reaction mixture was concentrated to dryness. The resulting residue was dissolved in methanol (15 ml) and 1N hydrochloric acid (1.5 ml) and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated to dryness and then the residue was extracted with methylene chloride-water. The organic layer was washed with water, dried, and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel to give yellow amorphous powders (90 mg, 56%).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. concentrationThe reaction mixture was concentrated to dryness
  4. dissolutionThe resulting residue was dissolved in methanol (15 ml)
  5. concentrationThe reaction mixture was concentrated to dryness
  6. extractionthe residue was extracted with methylene chloride-water
  7. washThe organic layer was washed with water
  8. customdried
  9. customevaporated to dryness
  10. customThe resulting residue was purified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-c8ea2189ee6b4b61903cdd22a0f5e1ca
Quelldatensatz
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05162326

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