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

Trifluoroacetic acid → HCID 178456704, Verbindung

HRID 484813
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 484813
C([S:14][C:15]1[N:19]([CH2:20][C:21]#[CH:22])[N:18]=[N:17][N:16]=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O>>[CH2:20]([N:19]1[C:15]([SH:14])=[N:16][N:17]=[N:18]1)[C:21]#[CH:22]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 130511525-benzhydrylthio-1-(2-propynyl)-1H-tetrazole

Produkt 1

HCID 178456704HCID 178456704, VerbindungAusbeute 59,3 %

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A mixture of 5-benzhydrylthio-1-(2-propynyl)-1H-tetrazole (0.35 g), anisole (0.6 g) and trifluoroacetic acid (3.4 ml) was stirred for 30 minutes at 20° C. and then allowed to stand for 45 minutes. The reaction mixture was filtered and the filter cake was washed with isopropyl ether. The filtrate and the washing were combined and evaporated under reduced pressure. After the addition of the residue to a saturated aqueous solution of sodium bicarbonate precooled to 10° C., the resulting mixture was adjusted to pH 8.5 with 2N aqueous solution of sodium hydroxide and washed with ethyl acetate. The washed aqueous layer was adjusted to pH 2.5 with 10% hydrochloric acid under ice-cooling and then extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and evaporated to give 1-(2-propynyl)-1H-tetrazole-5-thiol (95 mg), which is decomposed from 60° to 71° C.

Aufarbeitung

  1. waitto stand for 45 minutes
  2. filtrationThe reaction mixture was filtered
  3. washthe filter cake was washed with isopropyl ether
  4. customevaporated under reduced pressure
  5. additionAfter the addition of the residue to a saturated aqueous solution of sodium bicarbonate
  6. customprecooled to 10° C.
  7. washwashed with ethyl acetate
  8. temperaturecooling
  9. extractionextracted with ethyl acetate
  10. washThe extract was washed with a saturated aqueous solution of sodium chloride
  11. dry with materialdried over magnesium sulfate
  12. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-4fa4a12ea36e4a57a1fcaac1b366fc64
Quelldatensatz
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04533738

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion