反应详情

温度

2.5 °C

A solution comprising the reaction mixture prepared by Example 8, which reaction mixture contained the methyl 2,6-dichloro-5-methoxy-pyrimidine-4-carboxylate (25 g, 0.1 mol), and dimethyl sulfoxide (DMSO) was prepared. To this solution was added, at 0-5° C., a solution of ammonia in DMSO (2 eq). This mixture was stirred at the same 0-5° C. temperature for 10 to 15 minutes. Later, the mixture was diluted with ethyl acetate, and the resulting solid was filtered. The filtrate was washed with a brine solution. The organic layer was dried over sodium sulfate. Upon concentration, the crude product was obtained. The crude product was stirred in a minimum amount of ethyl acetate and filtered to obtain the pure compound. The resulting filtrate, after concentration, was column purified. This produced the title compound (11 g, 50% yield): mp 158° C.; 1H NMR (DMSO-d6) δ 3.71 (s, 3H), 3.86 (s, 3H), 7.65 (brs, 1H), 8.01 (brs, 1H).

1. customwas prepared
2. additionTo this solution was added, at 0-5° C.
3. filtrationthe resulting solid was filtered
4. washThe filtrate was washed with a brine solution
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationUpon concentration
7. customthe crude product was obtained
8. filtrationfiltered
9. customto obtain the pure compound
10. concentrationThe resulting filtrate, after concentration
11. custompurified