Table 5. Metallation of 12b followed by iodination reaction to give 13b. Complex T (°C) (%)[c] 1 25 n. r. 1 or 2 1:1 2 101 n. r. 3 25 n. r. [Mg][a] 1:1 4 101 42 5 25 10 1:1 6 101 33 9 7 25 8 1:2 8 101 31 9 25 12 1:1 10 101 56 10 11 25 14 1:2 12 101 55 [a] [Mg] corresponds to the complex [Mg{N(SiMe3)(Dipp)}(nBu)] made in situ. [b] Stoichiometric ratio between the substrate and the complex respectively. [c] Yield was calculated from 1H NMR spectra using 1,10-phenanthroline as internal standard. n.r. stands for no reaction. References
Table 5. Metallation of 12b followed by iodination reaction to give 13b. Complex T (°C) (%)[c] 1 1 or 2 1:1 25 n. r. 2 101 n. r. 3 [Mg][a] 1:1 25 n. r. 4 101 42 5 9 1:1 25 10 6 101 33 7 1:2 25 8 8 101 31 9 10 1:1 25 12 10 101 56 11 1:2 25 14 12 101 55 [a] [Mg] corresponds to the complex [Mg{N(SiMe3)(Dipp)}(nBu)] made in situ. [b] Stoichiometric ratio between the substrate and the complex respectively. [c] Yield was calculated from 1H NMR spectra using 1,10-phenanthroline as internal standard. n.r. stands for no reaction. References
1._General_procedures.docx