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Intermediate 8: 6-Bromo-5-chlo H)-one A mixture of 2-amino-5-bromo-4-chlorophenol (Intermediate 7, 8.4 g, 37.8 mmol), N,N-carbonyldiimidazole (12.2 g, 75.6 mmol) in THF (250 mL), was heated at 80 °C for 3 h. The solvent was removed under vacuum and the residue purified by column chromatography (silica: 200 - 400 mesh, 100 g) eluting with petroleum ether/ ethyl acetate from 9:1 to 5:1 ) to give 6-bromo-5-chlorobenzo[d]oxazol-2(3H)-one as an orange solid (7.7 g, 82percent). LCMS (A): Rt 1.49 min, MH+ 248/250.
methyl 3-(6-bromo-5-chloro-2-oxobenzo[d]oxazol-3(2H)-yl)propanoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
62%
With potassium carbonate; In acetonitrile; at 70℃; for 16h;
Methyl 3-(6-bromo-5-chloro-2-oxobenzo[d]oxazol-3(2H)- A mixture of 6-bromo-5-chlorobenzo[d]oxazol-2(3H)-one (Intermediate 8, 7.7 g, 31 mmol), <strong>[3395-91-3]methyl 3-bromopropanoate</strong> (6.2 g, 37 mmol), potassium carbonate (8.5 g, 62 mmol) in acetonitrile (200 mL), was stirred at 70 C for 16 h, the solvent was evaporated under vacuum, the residue purified by column chromatography (silica:200 - 400 mesh, 50 g) eluting with petroleum ether/ ethyl acetate 4:1 to give methyl 3-(6-bromo-5-chloro-2-oxobenzo[d]oxazol-3(2H)-yl)propanoate as an orange solid (6.2 g, 62%). LCMS (A): Rt 1.66 min, MH+ =334/336.
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