Boron Trichloride → Trimethylsilyl-cyclopentadienyl-dichloroborane

HRID 2230004

反応式

HRID 2230004 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 131722197Trimethylsilyl-cyclopentadienyl-dichloroborane収率 84.7%

実験手順

16 g (0.076 mole) of compound 1 were placed in a round bottom flask which was equipped with a dry ice cooling bath. 8.9 g (0.076 mole) BCl3 were condensed at −78° C. in a Schlenk tube and thereafter were added drop-wise to the round bottom flask over a period of 5 minutes. The reaction mixture was slowly heated to room temperature over 1 hour and was then maintained at 55 to 60° C. for a further 2 hours. All the volatile compounds were removed under vacuum (3 mm Hg=4 mbar). Subsequent distillation at 39° C. and 0.012 mbar gave 14.1 g of compound 2 (85% of the theoretical yield). The 1H NMR results agreed with the literature data and showed that a series of isomers had been produced (see J. Organometallic Chem. 169 (1979), 327). 11B NMR (64.2 MHz, C6D6): δ+31.5.

後処理

  1. customwhich was equipped with a dry ice cooling bath
  2. customcondensed at −78° C. in a Schlenk tube
  3. additionwere added drop-wise to the round bottom flask over a period of 5 minutes
  4. temperaturewas then maintained at 55 to 60° C. for a further 2 hours
  5. customAll the volatile compounds were removed under vacuum (3 mm Hg=4 mbar)
  6. distillationSubsequent distillation at 39° C.

出典と根拠

ORDレコード
ord-64a39234bca240ec893688d397b4c3f1
出典データセット
uspto-grants-2002_07
特許番号
US06423659B1

関連ノート

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