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