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Methanol → (R)-2-Bromo-1-phenylethanol

HRID 1635609
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1635609
[Br:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].CO>O1CCCC1>[Br:1][CH2:2][C@H:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 887MethanolHCID 6259Phenacyl bromide

Produkt 1

HCID 52694(R)-2-Bromo-1-phenylethanolAusbeute 84,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

(S)-2-amino-2-cyclohexyl-1,1-bis-(4-methoxyphenyl)ethanol (71.2 mg, 0.2 mmol), dry tetrahydrofuran (2 mL) and borane dimethylsulfide complex (1 00 μL, 1.0 mmol) were added to a dry flask under at atmosphere of nitrogen. The mixture was stirred at room temperature for 1.5 hours to form (R)-4-cyclohexyl-5,5-bis-(4-methoxy)phenyl-1,3,2-oxazaborolidine. A solution of bromoacetophenone (199 mg, 1.0 mmol) in dry tetrahydrofuran (4 mL) was added to the borane/(R)-4-cyclohexyl-5,5-bis-(4-methoxy)phenyl-1,3,2-oxazaborolidine complex at the rate of 9 mL/hr by means of a syringe pump. The resulting mixture was stirred at room temperature for an additional 1.5 hours. Methanol was added to quench the reaction and then the solvent was removed by evaporation. The resulting residue was chromatographed on silica gel (hexane/ethyl acetate, 25:1) and combination of the like fractions followed by removal of the solvent gave (S)-2-bromo-1-phenylethanol (170 mg, 96.6% ee). The enantiomeric excess was measured by HPLC (Chiralcel OD-H column, mobile phase, hexane/2-propanol 9:1, flow rate=0.7 mL/min).

Aufarbeitung

  1. customto quench
  2. customthe reaction
  3. customthe solvent was removed by evaporation
  4. customThe resulting residue was chromatographed on silica gel (hexane/ethyl acetate, 25:1) and combination of the like fractions
  5. customfollowed by removal of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-9a88feb2506d4b4aba94a3164e081bd4
Quelldatensatz
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06509472B2

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