Potassium Bromide → HCID 10221166, compound

Participants

Reaction Steps

A solution of diethylphosphonate 17 (160 mg; 0.57 mmol) in trimethylsilylbromide (4 ml) was refluxed overnight. The solvent/reagent was removed in vacuo and the residue was dissolved in 3 ml of 1N NaOH and washed with 2×1 ml of ether. The aqueous layer was acidified to pH 1 with 6N HCl and the precipitate which was formed was collected and washed with cold water, methanol and ether. The product was obtained as a white solid, mp 186° C. (dec) (80 mg; 60%). 1H NMR (D20): δ 3.06 (d, 2H, J=20.3 Hz); 6.54 (d, 1H, J=3.32 Hz); 7.12 (dd, 1H, J=2.03, 8.89 Hz); 7.36 (d, 1H, J=2.03 Hz); 7.89 (d, 1H, j=8.80 Hz). IR (KBr): 2931, 2828, 2360, 2309, 1658, 1643, 1532, 1406, 1224, 1147, 1093 cm-1. Anal. Calc' d for C10H9NO4ClP: C, 43.89; H, 3.32; N, 5.12. Found: C, 43.69; H, 3.41; N, 5.02.

Provenance & Evidence