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

Ethanethiol → 3-Methoxy-4-(methylsulfanyl)phenol

HRID 1279639
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1279639
[CH2:1]([O:8]CC1C=CC=CC=1)[C:2]1C=CC=[CH:4][CH:3]=1.[CH2:16]([SH:18])C.B(F)(F)F.C[CH2:24][O:25][CH2:26][CH3:27]>C(Cl)Cl>[CH3:24][O:25][C:26]1[CH:27]=[C:1]([OH:8])[CH:2]=[CH:3][C:4]=1[S:18][CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6343EthanethiolHCID 7657Dibenzyl etherHCID 8000Boron trifluoride etherate

Produkt 1

HCID 218771303-Methoxy-4-(methylsulfanyl)phenolAusbeute 28 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The benzylether from stage (iii) (9.27 g, 39.5 mmol) was dissolved in DCM (5 mL), ethanethiol (5 mL) and BF3.OEt2 (5 mL, 39.5 mol) were then added at room temperature under a nitrogen atmosphere. The mixture was stirred overnight before the reaction was quenched with hydrochloric acid (2 M) and stirred for a further 30 mins. The mixture was then basified by the addition of sodium hydroxide (2 M) until pH 10 was attained. The mixture was then washed with ethyl acetate (3×50 mL). The aqueous layer was reacidified by the addition of hydrochloric acid (2 M) to pH 1 and extracted with ethyl acetate (4×50 mL). The extracts were combined, dried (MgSO4) and evaporated to an oil. Purification by flash chromatography [SiO2; EtOAc/ pentane (1:9→1:4)] afforded the desired phenol compound as a colourless solid (1.73 g, 28%); δH(CDCI3, 400 MHz) 2.21 (3 H, s), 3.70 (3 H, s), 6.30 (1 H, d), 6.35 (1 H, s), 6.96 (1 H, d), 9.39 (1 H, brs)

Aufarbeitung

  1. customwas quenched with hydrochloric acid (2 M)
  2. stirringstirred for a further 30 mins
  3. additionThe mixture was then basified by the addition of sodium hydroxide (2 M) until pH 10
  4. washThe mixture was then washed with ethyl acetate (3×50 mL)
  5. additionThe aqueous layer was reacidified by the addition of hydrochloric acid (2 M) to pH 1
  6. extractionextracted with ethyl acetate (4×50 mL)
  7. dry with materialdried (MgSO4)
  8. customevaporated to an oil
  9. customPurification by flash chromatography [SiO2; EtOAc/ pentane (1:9→1:4)]

Quellen und Nachweise

ORD-Eintrag
ord-7fbc993ea7484477afab05404781d4c2
Quelldatensatz
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06448293B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion