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Magnesium bromide diethyl etherate → Phytanyl Bromide

HRID 1478959
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1478959
CCOCC.[Mg+2].[Br-:7].[Br-].S(O[CH2:14][CH2:15][CH:16]([CH2:18][CH2:19][CH2:20][CH:21]([CH2:23][CH2:24][CH2:25][CH:26]([CH2:28][CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH3:27])[CH3:22])[CH3:17])(=O)(=O)C>C(OCC)C>[CH2:14]([Br:7])[CH2:15][CH:16]([CH2:18][CH2:19][CH2:20][CH:21]([CH2:23][CH2:24][CH2:25][CH:26]([CH2:28][CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH3:27])[CH3:22])[CH3:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 9903262Magnesium bromide diethyl etherateHCID 60047967Phytanyl Mesylate

Produkt 1

HCID 10808570Phytanyl BromideAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a suspension of magnesium bromide diethyl etherate (25.9 g, 100.3 mmol) in anhydrous diethyl ether (250 mL) under nitrogen at room temperature was added a solution of phytanyl mesylate (18.9 g, 50.2 mmol) in anhydrous diethyl ether (200 mL) dropwise over 15 minutes. The resulting slurry was stirred for 72 hours at room temperature. Upon completion, the reaction mixture was cooled to 0° C. and ice cold water was added dropwise until all solid dissolved and bubbling stopped. Diethyl ether (300 mL) was added, and the organic and aqueous layers separated. The aqueous layer was back-extracted with diethyl ether (200 mL). The combined diethyl ether extracts were dried on MgSO4, filtered, and concentrated. The resulting oil was purified by column chromatography (column 10″L×2″W; eluted with 100% hexanes) to afford the product as a pale yellow oil (16.3 g, 90%).

Aufarbeitung

  1. temperatureUpon completion, the reaction mixture was cooled to 0° C.
  2. additionice cold water was added dropwise until all solid
  3. dissolutiondissolved
  4. custombubbling
  5. additionDiethyl ether (300 mL) was added
  6. customthe organic and aqueous layers separated
  7. extractionThe aqueous layer was back-extracted with diethyl ether (200 mL)
  8. dry with materialThe combined diethyl ether extracts were dried on MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe resulting oil was purified by column chromatography (column 10″L×2″W; eluted with 100% hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-fa7076f5d1434de49536bbbb443390bd
Quelldatensatz
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09404127B2

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