反应详情

To a solution of 4-hydroxy-2-(pyridin-2-yl)pyrimidine-5-carboxylic acid (10-c) (10 g, 46 mmol) in toluene (150 ml) was added DPPA (13.94 g, 50.6 mmol), Et3N (9.31, 92.1 mmol) and benzyl alcohol (14.93 g, 0.14 mol). The resulting mixture was heated at reflux overnight. Then the mixture was concentrated under vacuum and the residue was purified on silica gel chromatography with the eluent of petroleum ether/ethyl acetate=1/5, v/v, (Rf=0.3) to afford the crude compound 10-d (3.2 g). The sample delivered was re-purified on prep-HPLC. 1H NMR (DMSO-d6, 300 MHz): δ 8.73 (m, 1H), 8.40 (m, 2H), 8.00 (m, 1H), 7.37 (m, 6H), 5.19 (s, 1H). (M+H)+=323.1.

1. temperatureThe resulting mixture was heated
2. temperatureat reflux overnight
3. concentrationThen the mixture was concentrated under vacuum
4. customthe residue was purified on silica gel chromatography with the eluent of petroleum ether/ethyl acetate=1/5
5. customv/v, (Rf=0.3) to afford the crude compound 10-d (3.2 g)
6. customThe sample delivered was re-purified on prep-HPLC