反应详情

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.

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