反应详情

温度

110 °C

A suspension of 0.36 g (1 mmol) of 8-benzenesulphonyl-2-methyl-7-methylsulphanyl-3H-pyrazolo[1,5-a][1,3,5]triazin-4-one in 20 ml of POCl3 was treated with 0.12 ml (1.5 mmol) of pyridine and heated 110° C. for 3 hrs. The reaction solution was cooled to RT and evaporated. The residue was dried azeotropically twice with 50 ml of toluene each time. The thus-obtained residue was taken in 10 ml of 2N methylamine in tetrahydrofuran and stirred at room temperature for 4 hrs. The reaction solution was evaporated and partitioned between H2O and AcOEt. The organic phase was washed with H2O and sat. NaCl solution, dried (MgSO4), filtered and evaporated. Chromatography (SiO2, AcOEt/hexane 1:1) yielded 0.28 g (80%) of (8-benzenesulphonyl-2-methyl-7-methylsulphanyl-pyrazolo[1,5-a][1,3,5]triazin-4-yl)-methylamine as white crystals, m.p. 285° (dec).

1. temperatureThe reaction solution was cooled to RT
2. customevaporated
3. dry with materialThe residue was dried azeotropically twice with 50 ml of toluene each time
4. customThe reaction solution was evaporated
5. custompartitioned between H2O and AcOEt
6. washThe organic phase was washed with H2O and sat. NaCl solution
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated