反应详情

(5R)-3-(3-Fluoro-4-{6-[(5S)-5-(hydroxymethyl)-4,5-dihydroisoxazol-3-yl]pyridin-3-yl}phenyl)-5-(1H-1,2,3-triazol-1-ylmethyl)-1,3-oxazolidin-2-one (Example 1, 0.25 g, 0.57 mmol), 4-(dimethylamino)butanoic acid hydrochloride salt (0.24 g, 1.43 mmol), 4-dimethylaminopyridine (0.02 g, 0.16 mmol), and 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.25 g, 1.30 mmol) were combined in DMF (4 ml), The suspension was allowed to stir for one hour at room temperature resulting in a clear solution. The mixture was then concentrated in vacuo, suspended in ethyl acetate:acetonitrile (1:1) and filtered. The solids were dissolved in a minimum amount of methanol and submitted directly to purification via chromatography (silica gel, 1 to 20% methanol in dichloromethane). Evaporation of the product containing fractions and trituration of the resulting solid with diethyl ether yielded the title compound as a white solid (0.195 g), melting point: 148° C.

1. customresulting in a clear solution
2. concentrationThe mixture was then concentrated in vacuo
3. filtrationfiltered
4. dissolutionThe solids were dissolved in a minimum amount of methanol
5. customsubmitted directly to purification via chromatography (silica gel, 1 to 20% methanol in dichloromethane)
6. customEvaporation of the product
7. additioncontaining fractions and trituration of the resulting solid with diethyl ether