反应详情

温度

35 °C

3-Methyl-2-pyridinamine (431 g, 4.0 mol) was dissolved in dichloromethane (700 ml) and 4-(2-bromoethyl)benzenesulfonyl chloride (340 g, 1.33 mol) was added at room temperature. After 1 h at 20° C., the solution was heated to 35° C. for 2 h. Excess dilute hydrochloric acid was added and the phases separate& After washing once with water, the organic phase was dried with MgSO4 and treated with decolorizing carbon. The solvent was evaporated and warm methanol added to the residue, which crystallized. The material was collected and recrystallized from toluene. Yield 178 g. A further crop of 36 g was obtained by workup of the mother liquor. Total yield 45%.

1. washthe phases separate& After washing once with water
2. dry with materialthe organic phase was dried with MgSO4
3. additiontreated with decolorizing carbon
4. customThe solvent was evaporated
5. temperaturewarm methanol
6. additionadded to the residue, which
7. customcrystallized
8. customThe material was collected
9. customrecrystallized from toluene
10. customA further crop of 36 g was obtained by workup of the mother liquor