反应详情

温度

60 °C

A mixture of 17 parts of 5-methoxy-2-pyridinamine, 61 parts of phosphoryl chloride and 348 parts of methylbenzene was stirred for 2 hours at 60° C. 18 Parts of 3-acetyl-4,5-dihydro-2(3H)-furanone were added and the reaction mixture was stirred overnight at 90° C. The whole was poured into crushed ice and treated with ammonium hydroxide. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was stirred in a mixture of hexane and ethyl acetate (50:50 by volume). The precipitated product was filtered off and dried, yielding 10 parts (30.4%) of 3-(2-chloroethyl)-7-methoxy-2-methyl-4H-pyrido-[1,2-a]pyrimidin-4-one; mp. 150° C. (intermediate 3)

1. stirringthe reaction mixture was stirred overnight at 90° C
2. additionThe whole was poured
3. custominto crushed ice
4. extractionThe product was extracted with trichloromethane
5. customThe extract was dried
6. filtrationfiltered
7. customevaporated
8. stirringThe residue was stirred in a mixture of hexane and ethyl acetate (50:50 by volume)
9. filtrationThe precipitated product was filtered off
10. customdried