StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

HCID 13784978, Verbindung → HCID 14126642, Verbindung

HRID 329445
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 329445
[CH3:1][O:2][C:3]([CH:5]([C:7]1[CH:8]=[CH:9][C:10]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:11]([CH2:13][C:14](OC)=[O:15])[CH:12]=1)[CH3:6])=[O:4]>O>[O:15]=[C:14]1[C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[S:18][C:10]2[CH:9]=[CH:8][C:7]([CH:5]([CH3:6])[C:3]([O:2][CH3:1])=[O:4])=[CH:12][C:11]=2[CH2:13]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 13784978HCID 13784978, Verbindung

Produkt 1

HCID 14126642HCID 14126642, VerbindungAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 0.5 g of methyl 5-(1-methoxycarbonylethyl)-2-phenylthiophenylacetate [dicarboxylic acid ester] obtained in Example 1-(3) and 5.3 g of polyphosphoric acid (116%) was stirred at a temperature of 60°-80° C. for 6 hours. The mixture was cooled, and to this was added a mixture of ice and water to decompose excessive polyphosphoric acid. The resulting mixture was extracted with ethyl acetate. The organic layer was separated and washed successively with saturated brine solution, aqueous saturated sodium hydrogen carbonate solution and saturated brine solution. The washed extract was dried over anhydrous sodium sulfate. The solvent was distilled off from the dried extract under reduced pressure, and then the residue was recrystallized from a mixture of benzene and hexane to obtain 0.4 g of methyl 2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionate (yield 89%), m.p. 81.0°-82.0° C.

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. additionto this was added
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed successively with saturated brine solution, aqueous saturated sodium hydrogen carbonate solution and saturated brine solution
  6. extractionThe washed extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled off from the dried
  9. extractionextract under reduced pressure
  10. customthe residue was recrystallized from a mixture of benzene and hexane

Quellen und Nachweise

ORD-Eintrag
ord-fc800309d0e64155937b8549eeb6bdef
Quelldatensatz
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04891433

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion