反应详情

温度

0 °C

A solution of 2.59 g (37.6 mmol) of sodium nitrite in 10 ml of water was added dropwise at 0° C. to a solution of 8.00 g (18.8 mmol) of the amine from Example 22A in 200 ml of concentrated hydrogen chloride solution. After the addition had ended, the mixture was stirred at 0° C. for 1 h and then at RT for 2 h. The reaction mixture was diluted with 1 N aqueous hydrogen chloride solution and extracted with dichloromethane. The organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by means of preparative HPLC. Yield: 5.83 g (70% of theory)

1. additionAfter the addition
2. waitat RT for 2 h
3. extractionextracted with dichloromethane
4. dry with materialThe organic phase was dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by means of preparative HPLC