Triethylamine → 9-Methoxymethyl-9-triethylsilyloxymethyl-fluorene

HRID 2416164

Reaktionsgleichung

Reaktionsgleichung von HRID 2416164
[CH3:1][O:2][CH2:3][C:4]1([CH2:17][OH:18])[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2.C(N(CC)CC)C.[CH2:26]([Si:28](Cl)([CH2:31][CH3:32])[CH2:29][CH3:30])[CH3:27]>ClCCl>[CH3:1][O:2][CH2:3][C:4]1([CH2:17][O:18][Si:28]([CH2:31][CH3:32])([CH2:29][CH3:30])[CH2:26][CH3:27])[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 13819ChlorotriethylsilaneHCID 226391039-(Methoxymethyl)-9H-fluorene-9-methanol

Produkt 1

HCID 226390909-Methoxymethyl-9-triethylsilyloxymethyl-fluoreneAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1 g of 9-methoxymethyl-9-hydroxymethyl-fluorene (4.2 mmol) was dissolved in 20 ml of dichloromethane. The solution was cooled in ice-water bath, and 0.87 ml of triethyl amine (6.2 mmol) was added thereto. After stirring for 5 minutes, 0.91 ml of triethylsilyl chloride (5.4 mmol) was added drop-wise, and the mixture was stirred for further 2 hours, followed by stirring at room temperature for 1 hour. The reaction mixture was washed with water, and the organic layer separated was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated to give 1.24 g of concentrate (yield 84%).

Aufarbeitung

  1. stirringthe mixture was stirred for further 2 hours
  2. stirringby stirring at room temperature for 1 hour
  3. washThe reaction mixture was washed with water
  4. customthe organic layer separated
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. filtrationAfter filtration
  7. customthe filtrate was evaporated
  8. customto give 1.24 g
  9. concentrationof concentrate (yield 84%)

Quellen und Nachweise

ORD-Eintrag
ord-7375db9db7c94fd999b11389e37dc825
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06822109B2

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