反应详情

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.

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.