反应详情

A mixture of 4-(4-fluoro-benzyl)-1-hydroxy-3-oxo-6-trifluoromethyl-3,4-dihydro-4,4a-diaza-fluorene-2-carboxylic acid methyl ester (compound 43 d) (100 mg, 0.23 mmol), L-alanine (205 mg, 2.3 mmol) and sodium methoxide (99 mg, 1.84 mmol) in 2-methoxyethanol (3.5 mL) was microwaved at 150° C. for 2 h and concentrated. Residue was dissolved in water (80 mL), acidified to pH=3-4 using 1 N HCl solution and extracted with EtOAc. Organic layer was washed with brine, dried over MgSO4, filtered and concentrated. Crude product was purified by silica gel chromatography (15%-70% EtOAc (with 0.075% HOAc)/hexanes (with 0.1% HOAc)) to provide the title compound 34 mg. ESI (m/z): 490.03 (M−H)−.

1. customwas microwaved at 150° C. for 2 h
2. concentrationconcentrated
3. dissolutionResidue was dissolved in water (80 mL)
4. extractionextracted with EtOAc
5. washOrganic layer was washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customCrude product was purified by silica gel chromatography (15%-70% EtOAc (with 0.075% HOAc)/hexanes (with 0.1% HOAc))