反应详情

A mixture of 0.8 g of 2-{[(1-carbamoyl-1,2-dimethylpropyl)amino]methyl}-5-ethylnicotinic acid (2.7 mmol) and 0.56 g sodium acerate (6.8 mmol) in 10 mL acetic acid is warmed until homogeneous and cooled to room temperature. The solution is treated with 0.88 g bromine (5.45 mmol), and the reaction is stirred at 25° C. for 16 hours, then at 75° C. for three days. The reaction mixture is partitioned between CH2Cl2 and water, and the organic phase is dried and concentrated in vacuo. The residue is recrystallized from ethyl acetate-hexanes to afford 0.4 g of the title product having mp 172°-175° C.

1. temperatureis warmed until homogeneous and
2. waitat 75° C. for three days
3. customThe reaction mixture is partitioned between CH2Cl2 and water
4. customthe organic phase is dried
5. concentrationconcentrated in vacuo
6. customThe residue is recrystallized from ethyl acetate-hexanes