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

Iodine → 2-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethanol

HRID 2259767
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2259767
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][SH:12])=[CH:9][C:4]=2[O:3][CH2:2]1.[SH:13][CH2:14][CH2:15][OH:16].II.C(OCC)(=O)C>C(O)C.O>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][S:12][S:13][CH2:14][CH2:15][OH:16])=[CH:9][C:4]=2[O:3][CH2:2]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 807IodineHCID 15672-MercaptoethanolHCID 8857Ethyl AcetateHCID 158195122-(1,3-Benzodioxol-5-yl)ethanethiol

Produkt 1

HCID 190016232-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethanolAusbeute 23,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 962WaterLösungsmittel

Versuchsvorschrift

35 g of 2-(1,3-benzodioxol-5-yl)ethanethiol and 75 g of 2-mercaptoethanol were dissolved in 150 ml of ethanol, followed by the additional of 43 g of iodine. The obtained mixture was stirred at a room temperature for 30 minutes, followed by the addition of 2 l of ethyl acetate and 2 l of water. The mixture was separated into two phases. The ethyl acetate layer was washed with water twice, then with 1 l of a 1% aqueous solution of sodium hydrogensulfite twice and finally with water thrice, dried over anhydrous sodium sulfate and filtered. The filtrate was distilled to remove the solvent. The residue was purified by silica gel column chromatography (benzen/ethyl acetate=10:1) to obtain 11.5 g of the title compound as a colorless oil.

Aufarbeitung

  1. customThe mixture was separated into two phases
  2. washThe ethyl acetate layer was washed with water twice
  3. dry with materialwith 1 l of a 1% aqueous solution of sodium hydrogensulfite twice and finally with water thrice, dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. distillationThe filtrate was distilled
  6. customto remove the solvent
  7. customThe residue was purified by silica gel column chromatography (benzen/ethyl acetate=10:1)

Quellen und Nachweise

ORD-Eintrag
ord-86056ae00a084dc9be618c241ac2c769
Quelldatensatz
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05475024

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion