反应详情

836 mg (2.31 mmol) of the compound of Example 97A and 1.05 g (2.77 mmol) of HATU were dissolved in 14 ml of DMF, and 338 mg (2.77 mmol) of 4-N,N-dimethylaminopyridine (DMAP) were added slowly. 700 mg (2.31 mmol) of the compound of Example 11A were then added. The reaction mixture was stirred at RT for 3 h. About 200 ml of water were then added, and the mixture was extracted three times with in each case about 200 ml of ethyl acetate. The combined organic extracts were washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate, filtered and concentrated to dryness. The crude product obtained in this manner was purified by MPLC on about 100 g of silica gel with cyclohexane/ethyl acetate 50:50→0:100 as mobile phase. Evaporation of the product fractions and drying of the residue under high vacuum gave 966 mg (64% of theory) of the title compound.

1. extractionthe mixture was extracted three times with in each case about 200 ml of ethyl acetate
2. washThe combined organic extracts were washed with saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe crude product obtained in this manner
7. customwas purified by MPLC on about 100 g of silica gel with cyclohexane/ethyl acetate 50:50→0:100 as mobile phase
8. customEvaporation of the product fractions
9. customdrying of the residue under high vacuum