Boron Trichloride → Trimethylsilyl-cyclopentadienyl-dichloroborane

HRID 1977435

Reaktionsgleichung

Reaktionsgleichung von HRID 1977435
[CH3:1][Si:2]([C:5]1([Si](C)(C)C)[CH:9]=[CH:8][CH:7]=[CH:6]1)([CH3:4])[CH3:3].[B:14](Cl)([Cl:16])[Cl:15]>>[CH3:1][Si:2]([C:5]1([B:14]([Cl:16])[Cl:15])[CH:9]=[CH:8][CH:7]=[CH:6]1)([CH3:4])[CH3:3]

Komponenten

3

Edukt 2

HCID 25135Boron TrichlorideHCID 141813Silane, 2,4-cyclopentadien-1-ylidenebis(trimethyl-

Produkt 1

HCID 131722197Trimethylsilyl-cyclopentadienyl-dichloroboraneAusbeute 84,7 %

Versuchsvorschrift

16 g (0.076 mol) of the compound 1 were introduced into a round-bottomed flask equipped with a dry ice cooling bath. 8.9 g (0.076 mol) of BCl3 were condensed at −78° C. in a Schlenk tube and then added dropwise to the round-bottomed flask over a period of 5 minutes. The reaction mixture was warmed slowly to room temperature in the course of 1 hour and then kept at 55 to 60° C. for a further 2 hours. All the volatile compounds were removed in vacuo (3 mm Hg=4 mbar). Subsequent distillation at 39° C. under 0.012 mbar gave 14.1 g of the compound 2 (85% of the theoretical yield). The 1H-NMR agrees with the literature data and showed that a number of isomers had been prepared (cf. J. Organometallic Clhem. 169 (1979), 327). 11B-NMR (64.2 MHz, C6D6): δ=+31.5.

Aufarbeitung

  1. customequipped with a dry ice cooling bath
  2. customcondensed at −78° C. in a Schlenk tube
  3. additionadded dropwise to the round-bottomed flask over a period of 5 minutes
  4. customAll the volatile compounds were removed in vacuo (3 mm Hg=4 mbar)
  5. distillationSubsequent distillation at 39° C. under 0.012 mbar

Quellen und Nachweise

ORD-Eintrag
ord-8d0e07504c314a7aa678e0268afb39e7
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06232413B1

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