反应详情

温度

80 °C

To the solution of phosphorus oxychloride (65 mL, 0.70 mol) in trichloroethylene (46.5 mL) was added DMF (25 mL, 0.32 mol) slowly to keep the temperature between 5° C. to 10° C. The solution was then warmed up to room temperature before 6-hydroxy-2-(methylthio)-4(1H)-pyrimidinone (25 g, 0.16 mol) was added in portions. The resultant reaction mixture was heated at 80° C. overnight followed by concentration under vacuum. The resulting slurry like residue was poured into ice, stirred for 2 hours then filtered to afford the crude product. The crude product was further purified by recrystallization with hexane to afford 4,6-dichloro-2-(methylthio)-5-pyrimidinecarbaldehyde (21.3 g, 61%).

1. custombetween 5° C. to 10° C
2. additionwas added in portions
3. customThe resultant reaction mixture
4. concentrationfollowed by concentration under vacuum
5. additionThe resulting slurry like residue was poured into ice
6. filtrationthen filtered
7. customto afford the crude product
8. customThe crude product was further purified by recrystallization with hexane