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Sodium Chloride → HCID 131723900, Verbindung

HRID 413700
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 413700
[Si:1]([O:8][CH2:9][CH2:10][C:11]([C:14]1[C:19]([CH3:20])=[CH:18][C:17]([CH3:21])=[CH:16][C:15]=1[OH:22])([CH3:13])[CH3:12])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[H-].[Na+].[Br:25][CH2:26][CH2:27][CH2:28][C:29](Cl)=[O:30].[Cl-].[Na+]>O1CCCC1.O.CCOCC>[C:4]([Si:1]([CH3:2])([CH3:3])[O:8][CH2:9][CH2:10][C:11]([C:14]1[C:19]([CH3:20])=[CH:18][C:17]([CH3:21])=[CH:16][C:15]=1[OH:22])([CH3:12])[CH3:13])([CH3:7])([CH3:6])[CH3:5].[Br:25][CH2:26][CH2:27][CH2:28][C:29]([O-:30])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 702254-Bromobutyryl chlorideHCID 152992832-(4-((tert-Butyldimethylsilyl)oxy)-2-methylbutan-2-yl)-3,5-dimethylphenol

Produkt 1

HCID 131723900HCID 131723900, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 3283Diethyl EtherLösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To 3.22 g of 2-{3-(tert-butyldimethylsilyloxy)-1,1-dimethylpropyl}-3,5-dimethyl-phenol in solution in 60 cm3 of tetrahydrofuran, there are added, at 20° C. under an argon atmosphere and in small portions, 0.32 g of sodium hydride (at 75% in mineral oil), and then 15 minutes later 1.16 cm3 of 4-bromobutyryl chloride. After stirring for 40 minutes, 100 cm3 of ether, 10 cm3 of distilled water and 10 cm3 of a saturated aqueous sodium chloride solution are added. After stirring, the organic phase is decanted off, dried over magnesium sulfate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) to give a residue which is filtered on 75 g of silica (particle size 0.063-0.2 mm), eluting successively with cyclohexane and then with a cyclohexane/ethyl acetate mixture (90/10 by volume). 2 g of 2-{3-(tert-butyldimethyl-silyloxy)-1,1-dimethylpropyl}-3,5-dimethylphenol 4-bromobutyrate are thus obtained in the form of a colorless oil.

Aufarbeitung

  1. stirringAfter stirring
  2. customthe organic phase is decanted off
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  6. customto give a residue which
  7. filtrationis filtered on 75 g of silica (particle size 0.063-0.2 mm)
  8. washeluting successively with cyclohexane

Quellen und Nachweise

ORD-Eintrag
ord-e44194e8e29645fb8bdebdf64e8266a1
Quelldatensatz
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06569854B1

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