反应详情

The compound from Example 16A (320 mg, 0.74 mmol) was dissolved in 2.3 ml of DMF, HATU (309 mg, 0.81 mmol) and then 4-methylmorpholine (0.32 ml) were added, and the mixture was stirred at RT for 30 min. At −5° C., the compound of Example 7A (103 mg, 0.37 mmol) was then added and the mixture was stirred at RT for 16 h. A few milliliters of concentrated aqueous ammonia solution were then added. The mixture was stirred at RT for 15 min and then extracted with ethyl acetate. The organic phase was washed with conc. sodium chloride solution, dried over sodium sulphate, filtered and concentrated. The crude product was purified by preparative HPLC (Method 28). This gave 210 mg (purity 61%, 50% of theory) of the title compound which was used without further purification for the next synthesis step.

1. stirringthe mixture was stirred at RT for 16 h
2. stirringThe mixture was stirred at RT for 15 min
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with conc. sodium chloride solution
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was purified by preparative HPLC (Method 28)
9. customThis gave 210 mg (purity 61%, 50% of theory) of the title compound which was used without further purification for the next synthesis step