反应详情

350 g of methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate are suspended in 6.3 l of methylene chloride and 1 l of methanol. At room temperature there are added thereto 370 g of m-chloroperbenzoic acid and the mixture is stirred for a further 16 hours. The yellowish solution is subsequently extracted with 3 l of 2N soda solution. The aqueous phase is extracted with 1 l of methylene chloride. The combined organic phases are washed with 2 l of water and evaporated in vacuo. The crystalline residue is suspended in 1.5 l of ether while stirring. The pale yellowish crystals are filtered off under suction and washed with 0.5 l of ether. After drying at 40° in vacuo, there is obtained methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide.

1. additionAt room temperature there are added
2. extractionThe yellowish solution is subsequently extracted with 3 l of 2N soda solution
3. extractionThe aqueous phase is extracted with 1 l of methylene chloride
4. washThe combined organic phases are washed with 2 l of water
5. customevaporated in vacuo
6. filtrationThe pale yellowish crystals are filtered off under suction
7. washwashed with 0.5 l of ether
8. customAfter drying at 40° in vacuo