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Cyclobutanone → 1-Benzylcyclobutan-1-ol

HRID 1180725
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1180725
[C:1]1(=[O:5])[CH2:4][CH2:3][CH2:2]1.[CH2:6]([Mg]Cl)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>O1CCCC1.C(OCC)C>[CH2:6]([C:1]1([OH:5])[CH2:4][CH2:3][CH2:2]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 14496CyclobutanoneHCID 178418336HCID 178418336, Verbindung

Produkt 1

HCID 5618371-Benzylcyclobutan-1-olAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To 3.00 g (42.80 mmol) of cyclobutanone in 143 mL of tetrahydrofuran at 0° C. was added 51.36 mL (51.36 mmol) of a 1 M solution of benzyl magnesium chloride in diethyl ether and the mixture was allowed to warm to RT and stirred for 20 h. The reaction was quenched with methanol, followed by water. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give 6.52 g (94%) of 1-benzylcyclobutanol. Then, 1.90 g (11.69 mmol) of the compound was dissolved in 12 mL of toluene and 2.00 g (11.69 mmol) of methyl(2S)-2-isocyanatohexanoate was added. The mixture was heated at 85° C. for 3 d. The solution was concentrated and the residue was purified by silica gel column chromatography eluting with an ethyl acetate:hexanes solution (1:6) to give 2.44 g (63%) of methyl (2S)-2-({[(1-benzylcyclobutyl)oxy]carbonyl}amino)hexanoate. Rf=0.30 (1:4 ethyl acetate:hexanes); 1H NMR (300 MHz, DMSO-d6) δ 7.48 (d, J=8 Hz, 1H), 7.29-7.13 (m, 5H), 4.02-3.94 (m, 1H), 3.64 (s, 3H), 3.16 (ABq, JAB=16 Hz, Δ84 AB=12 Hz, 2H), 2.22-2.02 (m, 4H), 1.82-1.44 (m, 4H), 1.36-1.18 (m, 4H), 0.86 (t, J=7 Hz, 3H).

Aufarbeitung

  1. customThe reaction was quenched with methanol
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated sodium chloride
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-9a0dd51f9e1e4231ad9ad846001ab115
Quelldatensatz
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07282512B2

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