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 (100 mg, 0.23 mmol) and sodium glycinate (224 mg, 2.3 mmol) in 2-methoxyethanol (3.3 mL) was microwaved at 150° C. for 1 h and concentrated. Residue was dissolved in water (80 mL) and acidified to pH=3-4 using 1 N HCl solution. Precipitate was collected and rinsed with water. Solid was then dissolved in EtOAc, dried over MgSO4, filtered and concentrated. Crude product was triturated in MeOH (3 mL) and solid was collected and dried in vacuo to provide the title compound 62 mg. ESI (m/z): 476.01 (M−H)−

1. customwas microwaved at 150° C. for 1 h
2. concentrationconcentrated
3. dissolutionResidue was dissolved in water (80 mL)
4. customPrecipitate was collected
5. washrinsed with water
6. dissolutionSolid was then dissolved in EtOAc
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customCrude product was triturated in MeOH (3 mL)
11. customsolid was collected
12. customdried in vacuo