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

Sodium Hydroxide → HCID 19759911, Verbindung

HRID 1586856
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1586856
[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:4]=2[CH:3]=[C:2]1[C:9]([O:11]C)=[O:10].[OH-].[Na+]>C1COCC1.O>[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:4]=2[CH:3]=[C:2]1[C:9]([OH:11])=[O:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 19759902Methyl 4,5-dihydrothieno[2,3-b]thiophene-2-carboxylate

Produkt 1

HCID 19759911HCID 19759911, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Methyl 4,5-dihydrothieno[2,3-b]thiophene-2-carboxylate (9.5 g, 50 mmol) was dissolved in 200 mL THF followed by treatment with 100 mL of 20% sodium hydroxide and stirred overnight. THF was removed in vacuo to give a dark residue. The residue was taken up in water and extracted with ethyl acetate two times. The aqueous phase was then acidified to pH<1 with conc. HCl and extracted 3×200 mL ethyl acetate. The combined extracts were washed with: 1× water, 2× brine followed by drying over magnesium sulfate. The solution was filtered and the solvent evaporated to give the title compound as a solid (8.1 g). 1H NMR (300 MHz,DMSO-d6) d 2.5(t,2H), 2.8(t,2H), 7.5(s,1H), 12.8(bs,1H exch).

Aufarbeitung

  1. customTHF was removed in vacuo
  2. customto give a dark residue
  3. extractionextracted with ethyl acetate two times
  4. extractionextracted 3×200 mL ethyl acetate
  5. washThe combined extracts were washed with: 1× water, 2× brine
  6. dry with materialby drying over magnesium sulfate
  7. filtrationThe solution was filtered
  8. customthe solvent evaporated

Quellen und Nachweise

ORD-Eintrag
ord-2788891232c04f32858dc1e6cedbb4d7
Quelldatensatz
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05216020

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion