反应详情

The title compound was synthesized by combinatorial chemistry technique. That is, to a solution of the compound obtained in Example 329 (2) in dichloromethane (43.8 μmol/ml) (1 ml) were added a solution of ethylamine hydrochloride in N,N-dimethylformamide (35.0 μmol/ml) (1 ml), a solution of diisopropylethylamine (35.0 μmol/ml) (1 ml) and a suspension of carbodiimide resin in dichloromethane (79.2 mg/ml, manufactured by Argonaut) (1 ml), and the mixture was stirred at room temperature overnight. The reaction mixture was filtered, and the filter cake was washed twice with dichloromethane (1 ml), and the filtrate was washed with a saturated aqueous sodium hydrogen carbonate solution (2 ml), and then washed twice with water (2 ml). The organic layer was passed through a filter containing magnesium sulfate, and the filter was washed twice with dichloromethane (1 ml), and the filtrate was concentrated. To the residue was added a 90% trifluoroacetic acid (2 ml), and the mixture was stirred at room temperature for 2 hours, and concentrated. The residue was dissolved in dichloromethane (2 ml), and excess amount of ion-exchange resin (Dowex 1-X8, OH-type) was added thereto, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was filtered, and the filter cake was washed twice with dichloromethane (1 ml), and the filtrate was concentrated to give the title compound (6 mg).

1. customThe title compound was synthesized by combinatorial chemistry technique
2. filtrationThe reaction mixture was filtered
3. washthe filter cake was washed twice with dichloromethane (1 ml)
4. washthe filtrate was washed with a saturated aqueous sodium hydrogen carbonate solution (2 ml)
5. washwashed twice with water (2 ml)
6. additioncontaining magnesium sulfate
7. washthe filter was washed twice with dichloromethane (1 ml)
8. concentrationthe filtrate was concentrated
9. additionTo the residue was added a 90% trifluoroacetic acid (2 ml)
10. stirringthe mixture was stirred at room temperature for 2 hours
11. concentrationconcentrated
12. dissolutionThe residue was dissolved in dichloromethane (2 ml)
13. additionexcess amount of ion-exchange resin (Dowex 1-X8, OH-type) was added
14. stirringthe mixture was stirred at room temperature for 1 hour
15. filtrationThe reaction mixture was filtered
16. washthe filter cake was washed twice with dichloromethane (1 ml)
17. concentrationthe filtrate was concentrated