反应详情

温度

0 °C

4.0 g of commercially available 6-aminoisoquinoline was suspended in 40 mL of concentrated hydrochloric acid (35%) with cooling at 0° C. To the suspension, 4.0 g of sodium nitrite was added in small portions, and the mixture was stirred for 30 minutes. This reaction solution was added dropwise at 0° C. to a mixed solution of 20 mL of acetic acid saturated with sulfite gas generated from sodium bisulfite and sulfuric acid, and 298 mg of copper chloride, and the mixture was stirred for 1 hour. The mixture was neutralized by the addition of a saturated aqueous solution of sodium bicarbonate, followed by extraction with dichloromethane (100 mL×2). The obtained organic layer was washed with saturated saline and then dried over anhydrous sodium sulfate. A dichloromethane solution obtained by filtration was used in the next reaction without being further purified because the compound of interest was unstable.

1. stirringthe mixture was stirred for 1 hour
2. extractionfollowed by extraction with dichloromethane (100 mL×2)
3. washThe obtained organic layer was washed with saturated saline
4. dry with materialdried over anhydrous sodium sulfate
5. customA dichloromethane solution obtained by filtration
6. customwas used in the next reaction
7. customwithout being further purified because the compound of interest