反应详情

3.5 g of crude methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide are dissolved in 100 ml of methylene chloride and 50 ml of tetrahydrofuran. At 0° there are added thereto 2.2 g of N-methylmorpholine and subsequently 1.45 ml of methyl chloroformate in 20 ml of methylene chloride. The mixture is stirred at 0° for 1 hour and then at room temperature for 2 hours and thereupon treated with a small amount of methanol and water. The organic phase is separated, dried and evaporated. The residue is recrystallized from methylene chloride and ether, there being obtained pure dimethyl 6-[(p-tolylsulfonyl)oxy]-2,4-pyrimidinedicarbamate-3-oxide of melting point 178°-179°.

1. additionAt 0° there are added
2. waitat room temperature for 2 hours
3. customThe organic phase is separated
4. customdried
5. customevaporated
6. customThe residue is recrystallized from methylene chloride and ether, there