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Diethanolamine → 4-Chloro-3-(methylthio)phenol

HRID 724271
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 724271
B(Br)(Br)Br.[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([O:12]C)=[CH:8][C:7]=1[S:14][CH3:15].N(CCO)CCO>ClCCl>[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][C:7]=1[S:14][CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8113DiethanolamineHCID 25134Boron tribromideHCID 21877168(2-Chloro-5-methoxyphenyl)(methyl)sulfane

Produkt 1

HCID 218771864-Chloro-3-(methylthio)phenolAusbeute 80,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

Boron tribromide (1M in dichloromethane, 31 ml, 31 mmol) was added dropwise to a solution of 1-chloro-4-methoxy-2-(methylsulfanyl)benzene (2.88 g, 15 mmol) in dichloromethane (80 ml) at 0° C. The mixture was allowed to warm to room temperature, stirred for 72 h then cooled to 0° C. A solution of diethanolamine (10 ml) in dichloromethane (20 ml) was added dropwise (Caution—strong exotherm!) and the mixture was stirred at ambient temperature for 15 min once addition was complete, then partitioned between dichloromethane and 2N hydrochloric acid. The organic phase was washed with water, dried over MgSO4 and the solvent removed under reduced pressure. The residue was purified by flash column chromatography using ethyl acetate:cyclohexane (10:90 to 85:15) as eluant to give 4-chloro-3-(methylsulfanyl)phenol (2.12 g) as a brown oil.

Aufarbeitung

  1. temperaturethen cooled to 0° C
  2. stirringthe mixture was stirred at ambient temperature for 15 min
  3. additiononce addition
  4. custompartitioned between dichloromethane and 2N hydrochloric acid
  5. washThe organic phase was washed with water
  6. dry with materialdried over MgSO4
  7. customthe solvent removed under reduced pressure
  8. customThe residue was purified by flash column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-68141703564d462bab8d2aa263b9ebcb
Quelldatensatz
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07141586B2

Notizen zur Reaktion

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