Bromotrimethylsilane → HCID 68593442, compound

Participants

Reaction Steps

Compound 47.1 (277 mg, 0.45 mmol) was dissovled in 4.5 mL anhydrous CH3CN and treated with TMSBr (0.9 mL, 6.8 mmol). The solution was stirred at rt for 3 h, and then concentrated under reduced pressure. The residue was dissolved in NH4OH, stirred for another 2 h, and concentrated under reduced pressure. The residue was subjected to a reverse phase HPLC to give compound 47.2 (97 mg, 51% yield). 1H NMR (D2O, 300 MHz): δ 2.15-2.23 (m, 2H), 3.02 (s, 3H), 4.96 (s, 1H), 5.90-5.95 (m, 1H), 6.02 (d, 1H, J=1.2), 6.39 (m, 1H), 8.09 (s, 1H), 8.17 (s, 1H). 31PNMR: 11.34 ppm. LRMS [M−H]− C12H16N5O5P requires 340.1. Found 340.0.

Provenance & Evidence