反应详情

温度

70 °C

To a vessel containing a stir bar was added {[4-(5-bromo-6-chloro-pyridine-3-sulfonyl)-5-methylsulfanyl-thiophen-2-yl]-imino-methyl}-carbamic acid tert-butyl ester (0.035 g, 0.066 mmol), 4-aminomethylpyridine (0.015 g, 0.133 mmol), THF [3 mL]. The reaction vessel was sealed and heated to 70° C. for 18 hours, cooled to room temperature and concentrated in vacuo. The crude residue was dissolved in a solution of chloroform/trifluoroacetic acid (1/1) [2 mL] and was allowed to stir at room temperature for 2 hours. The reaction was concentrated in vacuo followed by reverse-phase HPLC [acetonitrile/water (0.01% TFA)] to give the title compound. ESI-MS (m/z): Calcd. for C17H16BrN5O2S3: 499.44 (M+H); found 498.0, 500.0.

1. additionTo a vessel containing a stir bar
2. customThe reaction vessel was sealed
3. temperaturecooled to room temperature
4. concentrationconcentrated in vacuo
5. dissolutionThe crude residue was dissolved in a solution of chloroform/trifluoroacetic acid (1/1) [2 mL]
6. concentrationThe reaction was concentrated in vacuo