反应详情

65 mg (0.16 mmol) of the compound of Example 9A, 68 mg (0.158 mmol) of the compound of Example 16A and 72 mg (0.19 mmol) of HATU were initially charged in 0.9 ml of DMF, 0.033 ml (0.19 mmol) of N,N-diisopropylethylamine were added and the mixture was stirred at RT for 1 h. The reaction was then stirred into 10 ml of 0.1 M aqueous sodium hydroxide solution. After 10 min of further stirring at RT, the precipitate formed was filtered off, washed with water and dried. The intermediate obtained in this manner was dissolved in 0.5 ml of trifluoroacetic acid and stirred at 80° C. for 6 h. The mixture was then concentrated under reduced pressure and the residue was purified by double preparative HPLC (Method 18). This gave 18 mg (19% of theory) of the title compound.

1. stirringAfter 10 min of further stirring at RT
2. customthe precipitate formed
3. filtrationwas filtered off
4. washwashed with water
5. customdried
6. customThe intermediate obtained in this manner
7. stirringstirred at 80° C. for 6 h
8. concentrationThe mixture was then concentrated under reduced pressure
9. customthe residue was purified by double preparative HPLC (Method 18)