反应详情

The ethyl methylphosphinate 2-4 (130 mg, 0.27 mmol) was dissolved in 5 ml of dioxane and treated with 2 ml of 5N NaOH. The mixture was heated at reflux overnight. The mixture was then concentrated under vacuum and the residue was treated with 2 ml of trifluoroacetic acid. The mixture was re-evaporated and the residue was purified by prep-HPLC to provide the product, 2-5 (80 mg, 64%). 1H NMR (CD3OD, 300 MHz,): δ 8.76 (m, 2H), 8.48 (m, 2H), 8.01 (m, 1H), 7.77 (m, 2H), 7.61 (m, 1H), 7.51 (m, 2H), 7.29 (m, 5H), 6.39 (s, 1H), 1.61 (d, 3H).

1. temperatureThe mixture was heated
2. temperatureat reflux overnight
3. concentrationThe mixture was then concentrated under vacuum
4. additionthe residue was treated with 2 ml of trifluoroacetic acid
5. customThe mixture was re-evaporated
6. customthe residue was purified by prep-HPLC