Sodium Carbonate → HCID 69230364, Verbindung

HRID 661770Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 661770
[H-].[K+].[C:3]([C:7]1[CH:8]=[CH:9][C:10]2[CH2:11][C:12]3[C:17]([C:18]=2[CH:19]=1)=[CH:16][C:15]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:14][CH:13]=3)([CH3:6])([CH3:5])[CH3:4].[CH2:24]([O:27][C:28]1[C:33]([C:34]([CH3:37])([CH3:36])[CH3:35])=[CH:32][C:31]([CH3:38])=[CH:30][C:29]=1[Si:39](Cl)([CH2:42][CH3:43])[CH2:40][CH3:41])[CH:25]=[CH2:26].C(=O)([O-])O.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>CCCCCC.C1COCC1.C1(C)C=CC=CC=1>[CH2:24]([O:27][C:28]1[C:33]([C:34]([CH3:35])([CH3:36])[CH3:37])=[CH:32][C:31]([CH3:38])=[CH:30][C:29]=1[Si:39]([CH:11]1[C:10]2[CH:9]=[CH:8][C:7]([C:3]([CH3:6])([CH3:5])[CH3:4])=[CH:19][C:18]=2[C:17]2[C:12]1=[CH:13][CH:14]=[C:15]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:16]=2)([CH2:40][CH3:41])[CH2:42][CH3:43])[CH:25]=[CH2:26]

Komponenten

9

Edukt 5

HCID 10340Sodium CarbonateHCID 82127Potassium hydride2×HCID 516892Sodium BicarbonateHCID 111404373,6-DI-Tert-butylfluoreneHCID 67206735(2-Allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilane

Produkt 1

HCID 69230364HCID 69230364, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 1140TolueneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel3×HCID 8058HexaneLösungsmittel

Versuchsvorschrift

There was washed 1.50 g (11.22 mmol) of potassium hydride having a purity of 30% by weight with each 3 mL of hexane three times in an atmosphere of nitrogen, and 18 mL of THF was added thereto. To the obtained THF slurry of potassium hydride, 2.50 g (8.98 mml) of 3,6-di-tert-butylfluorene was added dropwise at 0° C. using 18 mL of a THF solution thereof. The obtained mixture was stirred for 2 hours at a room temperature, and then 2.92 g (8.98 mmol) of (2-allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilane was added dropwise at −78° C. using 4 mL of a toluene solution thereof. The temperature of the obtained liquid reaction mixture was raised up to a room temperature, and the mixture was stirred for 2 hours. The mixture was added dropwise at 0° C. to a mixture of 18 mL of a 10% aqueous solution of sodium hydrogen carbonate and 18 mL of a 10% aqueous solution of sodium carbonate, and the resultant mixture was extracted with 10 mL of toluene. The obtained extract was dried over sodium sulfate, and dried extract was concentrated under a reduced pressure, thereby obtaining quantitatively (2-allyloxy-3-tert-butyl-5-methylphenyl)(3,6-di-tert-butylfluoren-9-yl)diethylsilane.

Aufarbeitung

  1. additionwas added
  2. customThe temperature of the obtained liquid reaction mixture
  3. temperaturewas raised up to a room temperature
  4. stirringthe mixture was stirred for 2 hours
  5. extractionthe resultant mixture was extracted with 10 mL of toluene
  6. extractionThe obtained extract
  7. dry with materialwas dried over sodium sulfate
  8. customdried
  9. extractionextract
  10. concentrationwas concentrated under a reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-292c8949cf154008a7589145cc64c0e7
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084559B2

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