反应详情

A solution of methyl 4-(1,3-dibenzyl-1,2,3,4-tetrahydro-2,4-dioxopyrimidin-5-yl)-2-hydroxy-4-oxobut-2-enoate (3a) (757 mg, 1.8 mmol) in dioxane (100 ml) was refluxed with 1N HCl (60 ml) for 4 h. The solution was evaporated to dryness. The resulting solid was recrystalized from hexane and ethyl acetate (3:1) to give 617 mg a pale yellow solid. Yield was 84.2%. Mp. 186-188° C. 1HNMR (DMSO-d6): 8.89 (s, 1H), 7.57 (s, 1H), 7.24-7.36 (m, 10H), 5.16 (s, 2H), 5.02 (s, 2H). 13CNMR (DMSO-d6): 186.1, 169.0, 163.2, 159.9, 151.1, 150.2, 136.5, 135.8, 128.7, 128.4, 128.0, 127.8, 127.6, 127.3, 107.7, 100.9, 52.8, 44.2. FAB-HRMS: [M+H]+ calcd. for C22H19N2O6 407.1243, found 407.1248.

1. customThe solution was evaporated to dryness
2. customThe resulting solid was recrystalized from hexane and ethyl acetate (3:1)