反应详情

温度

65 °C

Potassium hydroxide (8.4 g) was added to a solution of intermediate 2 (33 g) in dimethyl sulfoxide (150 ml). The mixture was stirred for 1 hour at 60-70 ° C. The mixture was cooled to 20° C. and iodomethane (21.3 g) was added dropwise. The reaction mixture was stirred overnight at RT. The mixture was poured out into water and extracted with toluene. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was crystallized from 4-methyl-2-pentanone and the precipitate was filtered off and dried, yielding 16 g (46%) of 2-(ethylthio)-5-(2-hydroxy-ethyl)-3,6-dimethyl-4(3H)-pyrimidinone (intermediate 3).

1. temperatureThe mixture was cooled to 20° C.
2. stirringThe reaction mixture was stirred overnight at RT
3. extractionextracted with toluene
4. customThe separated organic layer was dried
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was crystallized from 4-methyl-2-pentanone
8. filtrationthe precipitate was filtered off
9. customdried