反应详情

A mixture of 2-fluorobenzaldehyde (5 g, 40.28 mmol), urea (3.8 g, 61 mmol), ethylacetoaceate (5.24 g, 40.28 mmol), CuCl (0.4 g, 4 mmol), BF3.OEt2 (7 mL, 53 mmol), and glacial acetic acid (0.24 g, 4 mmol) in THF (80 mL) was refluxed for 18 h and then cooled to room temperature. The mixture was quenched with saturated NaHCO3 (50 mL), and EtOAc (100 mL) was added. The layers were separated and the organic layer with a white suspension was evaporated to give a white solid. The solid was suspended in toluene (100 mL) and stirred for 2 days at room temperature. The solid was filtered, washed with ether, and dried to give ethyl 4-(2-fluorophenyl)-1,2,3,4-tetrahydro-6-methyl-2-oxopyrimidine-5-carboxylate (9.9 g, 88%). Mass Spec. FIA MS 279 (M+1).

1. temperaturewas refluxed for 18 h
2. customThe mixture was quenched with saturated NaHCO3 (50 mL), and EtOAc (100 mL)
3. additionwas added
4. customThe layers were separated
5. customthe organic layer with a white suspension was evaporated
6. customto give a white solid
7. filtrationThe solid was filtered
8. washwashed with ether
9. customdried