反应详情

Iodotrimethylsilane (2.0 mL, 14.2 mmol) in 5 mL of dry CH2Cl2 was added dropwise to a solution of 11b1 (2.0 g, 3.55 mmol) and bis(trimethylsilyl)trifluoroacetamide (1.8 mL, 7.1 mmol) in 20 mL of dry CH2Cl2 at 0° C. under argon. Stirring was continued for 1 h at 0° C. and 1 h at room temperature. The solution was concentrated in vacuo. The residue was treated with 20 mL of MeCN/H2O (9:1) and 5 drops of conc. HCl for 30 min and concentrated in vacuo. Toluene (5 mL) was added and evaporated twice. On addition of Et2O solids separated, which were collected by filtration and washed with the same solvent to give, after drying over P2O5 in vacuo, 1.6 g of 12b as a white powder (88%). It was used without further purification. 1H NMR (DMSO-d6, 300 MHz) δ 2.6 (s, 3H), 6.6 (s, 1H), 7.24 (d, J=8.7 Hz, 2H), 7.75 (d, J=8.7 Hz, 2H). HRMS (M+H) calc, 503.8658; found, 503.8691.

1. concentrationThe solution was concentrated in vacuo
2. additionThe residue was treated with 20 mL of MeCN/H2O (9:1) and 5 drops of conc. HCl for 30 min
3. concentrationconcentrated in vacuo
4. additionToluene (5 mL) was added
5. customevaporated twice
6. additionOn addition of Et2O solids
7. customseparated
8. filtrationwhich were collected by filtration
9. washwashed with the same solvent
10. customto give
11. dry with materialafter drying over P2O5 in vacuo, 1.6 g of 12b as a white powder (88%)
12. customIt was used without further purification