反应详情

4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxylic acid, 30-ie, (545 mg, 2.5 mmol) in 5 ml of thionyl chloride was heated at reflux overnight. Then it was concentrated under vacuum and the residue was dissolved in 10 ml of dichloromethane. To the mixture was added 4-(amino(4-methoxyphenyl)methyl)phenylphosphinic acid hydrochloride (1-1-e, 782.5 mg, 2.5 mmol) and TEA (505 mg, 5 mmol) in 10 ml of dichloromethane at 0° C. The mixture was stirred for 3 hours and then it was washed with sat. NH4Cl. The organic layer was concentrated under vacuum and the residue was purified on prep-HPLC to provide the product 9-2 (150 mg, 12%). 1H NMR (CD3OD, 300 MHz,): δ 9.37 (m, 1H), 8.83 (s, 1H), 8.51 (m, 1H), 8.15 (m, 1H), 7.80 (m, 2H), 7.53 (m, 2H), 7.23 (m, 2H), 6.79 (m, 2H), 6.56 (s, 1H), 6.34 (s, 1H), 3.77 (s, 3H).

1. temperatureat reflux overnight
2. concentrationThen it was concentrated under vacuum
3. dissolutionthe residue was dissolved in 10 ml of dichloromethane
4. washit was washed with sat. NH4Cl
5. concentrationThe organic layer was concentrated under vacuum
6. customthe residue was purified on prep-HPLC