反应详情

To a solution of the compound of Example 8 (200 mg, 0.32 mmol) in dichloromethane (5 mL) and N,N-dimethylformamide (5 mL) were added excess amount of dimethylamine and bis-(2-oxo-3-oxazolidinyl)-phosphinic chloride (325.2 mg, 1.27 mmol), and the mixture was stirred at room temperature for 28 hours. To the reaction solution was added saturated aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate-toluene (1:1). The organic layer was dried over anhydrous magnesium sulfate, and then filtered and concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol/ammonia water=20/1/0 to 10/1/0 to 200/10/1 to 100/10/1). To the purified substance were added tetrahydrofuran and 1M hydrochloric acid (1 mL), and the mixture was concentrated. The resulting solid was suspended in diethyl ether, and then filtered to give the titled compound (139.0 mg, 72%).

1. extractionthe mixture was extracted with ethyl acetate-toluene (1:1)
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol/ammonia water=20/1/0 to 10/1/0 to 200/10/1 to 100/10/1)
6. additionTo the purified substance were added tetrahydrofuran and 1M hydrochloric acid (1 mL)
7. concentrationthe mixture was concentrated
8. filtrationfiltered