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

Sodium hydride → (R,Z)-2-(hex-3-enyl)oxirane

HRID 1432815
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1432815
[CH2:1]([OH:10])[C@H:2](O)[CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8].[H-].[Na+].C(C1C=CC(S(Cl)(=O)=O)=C(C(C)C)C=1C(C)C)(C)C>C1COCC1>[CH2:3]([C@@H:2]1[CH2:1][O:10]1)[CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 11514985Triisopropylbenzenesulfonyl chlorideHCID 58906721(R,Z)-oct-5-ene-1,2-diol

Produkt 1

HCID 58906753(R,Z)-2-(hex-3-enyl)oxirane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of (R,Z)-oct-5-ene-1,2-diol (8.50 g, 58.9 mmol) in THF (230 mL) at 0° C. was added NaH (60% dispersion in mineral oil, 7.06 g, 177 mmol) (7.06 g as dispersion). The mixture was warmed to ambient temperature and stirred for 40 min. The reaction was cooled to 0° C. and triisopropylbenzenesulfonyl chloride (20.7 g, 61.8 mmol) was added. The reaction was warmed to room temp, stirred for 1 h, quenched with H2O and extracted with Et2O. The organics were washed with brine, dried over MgSO4, filtered, and concentrated. Purification by silica gel chromatography (2% Et2O in pentane gradient to 8% Et2O in pentane) gave (R,Z)-2-(hex-3-enyl)oxirane. It was determiined that slight racemization occurred at this step (98% ee to 84% ee). In order to ensure optical purity the enantioenriched product was further resolved using Jacobsen's hydrolytic kinetic resolution (HKR, Step E). 1H NMR (400 MHz, CDCl3): δ 5.41 (1H, m), 5.35 (1H, m), 2.93 (1H, m), 2.75 (1H, dd, J=5.2, 4.4 Hz), 2.49 (1H, dd, J=5.2, 2.8 Hz), 2.20 (2H, q, J=6.8 Hz), 2.06 (2H, quin, 7.6 Hz); 1.59 (2H, m), 0.97 (3H, t, J=7.6 Hz).

Aufarbeitung

  1. temperatureThe reaction was cooled to 0° C.
  2. temperatureThe reaction was warmed to room temp
  3. stirringstirred for 1 h
  4. customquenched with H2O
  5. extractionextracted with Et2O
  6. washThe organics were washed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customPurification by silica gel chromatography (2% Et2O in pentane gradient to 8% Et2O in pentane)

Quellen und Nachweise

ORD-Eintrag
ord-caf523f482c54e79af7094c5e60aef4e
Quelldatensatz
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07612106B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion