反应详情

The intermediate, 6-(chloromethyl)-2-(1-methylethyl)-4(1H)pyrimidinone, was prepared according to Swiss patent 524617 from ethyl 4-chloroacetoacetate and isobutyramidine. m.p. 123°-125°. The intermediate chloromethyl compound (25 g) was stirred with 50 ml methanol at room temperature. To this mixture was added, dropwise, a solution of 25 g ammonium dimethyl phosphorodithioate dissolved in 500 ml methanol. The mixture was then heated to reflux for 6 hours, then the solvent was evaporated under reduced pressure yielding a solid. The solid was dissolved in dichloromethane and washed with water, separated, dried, and the solvent was evaporated. The remaining solid was recrystallized from toluene; yield: 15.9 g, m.p. 89°-93°.

1. additionTo this mixture was added
2. temperatureThe mixture was then heated
3. temperatureto reflux for 6 hours
4. customthe solvent was evaporated under reduced pressure
5. customyielding a solid
6. washwashed with water
7. customseparated
8. customdried
9. customthe solvent was evaporated
10. customThe remaining solid was recrystallized from toluene