反应详情

1.00 g (3.46 mmol) of the compound of Example 6A, 944 mg (3.46 mmol) of the compound of Example 23A and 1.58 g (4.15 mmol) of HATU were dissolved in 12.1 ml of anhydrous DMF, and 0.72 ml (4.15 mmol) of N,N-diisopropylethylamine was added. The reaction mixture was stirred at RT for 1 h and then stirred into 120 ml of 0.1 M aqueous sodium hydroxide solution. After a further 10 min of stirring at RT, the precipitate formed was filtered off and dried. This crude product was then separated into its components by preparative HPLC (Method 23). The product fractions were combined and concentrated to dryness on a rotary evaporator. The product obtained was suspended in a mixture of 10 ml of acetonitrile and 10 ml of water, made alkaline with a little saturated sodium bicarbonate solution and stirred at RT for 10 min. The solid was filtered off, washed with water and dried. This gave 1.12 g (69% of theory) of the title compound.

1. stirringAfter a further 10 min of stirring at RT
2. customthe precipitate formed
3. filtrationwas filtered off
4. customdried
5. customThis crude product was then separated into its components by preparative HPLC (Method 23)
6. concentrationconcentrated to dryness on a rotary evaporator
7. customThe product obtained
8. stirringstirred at RT for 10 min
9. filtrationThe solid was filtered off
10. washwashed with water
11. customdried