Reaction equation
[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]Participants
Procedure
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 agreed with the literature data and showed that a number of isomers had been prepared (cf. J. Organometallic Chem. 169 (1979), 327). 11B-NMR (64.2 MHz, C6D6): δ=+31.5.
Workup
- customequipped with a dry ice cooling bath
- customcondensed at -78° C. in a Schlenk tube
- additionadded dropwise to the round-bottomed flask over a period of 5 minutes
- customAll the volatile compounds were removed in vacuo (3 mm Hg=4 mbar)
- distillationSubsequent distillation at 39° C. under 0.012 mbar
Sources & evidence
- ORD record
- ord-008c3ca0a8cb42938e847a3edd21c8a3
- Source dataset
- uspto-grants-2000_12
- Patent number
- US06156857
Linked notes
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