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With pyridine; oxalyl dichloride; In dichloromethane; at 0 - 20℃; for 2h;Inert atmosphere;
C1COCOC1 ( 44.4 mL, 510.2 mmol) was added dropwise to the mixture of PR-13 (100.6 g, 374 mmol), <strong>[112253-70-0]2-amino-4-bromobenzamide</strong> (73.2 g, 340 mmol) and pyridine (760 mL) under nitrogen at 0C. The mixture was stirred for 2 hour at room temperature. The solvent was removed in vacuo. Saturated NaHC03 was added to the residue and the resulting mixture was extracted by ethyl acetate for three times. The combined organic layers were washed with saturated NaHC03, brine and dried over Na2S04. The solvent was removed in vacuo. The obtained residue was purified by chromatography (CH2Cl2:MeOH=50: l) resulting in an intermediate amide compound (50.6 g). Method A2; Rt: 1.15 min. m/z=:490.1 (M+Na)+ Exact mass: 467.1 A solution of the above obtained intermediate (50.61g), Na2C03 (34.5 lg. 325.6 mmol), H20 (300 mL) and CH3CH2OH (300 mL) was stirred for 3 hours at reflux. EtOH was removed in vacuo and the mixture was extracted with ethyl acetate (3 x 300 mL). The combined organic layers were dried over Na2S04 and concentrated in vacuo. The obtained residue was washed with t-butyl methyl ether resulting in compound QA-9 (39.2 g). Method A2; Rt: 1.37 min. m/z=:448.1 (M+H)+ Exact mass: 447.1
50.6 g
With pyridine; oxalyl dichloride; at 0 - 20℃; for 2h;Inert atmosphere;
C1COCOC1 ( 44.4 mL, 510.2 mmol) was added dropwise to the mixture of PR-13 (100.6 g, 374 mmol), <strong>[112253-70-0]2-amino-4-bromobenzamide</strong> (73.2 g, 340 mmol) and pyridine (760 mL) under nitrogen at 0C. The mixture was stirred for 2 hour at room temperature. The solvent was removed in vacuo. Saturated NaHC03 was added to the residue and the resulting mixture was extracted by ethyl acetate for three times. The combined organic layers were washed with saturated NaHC03, brine and dried over Na2S04. The solvent was removed in vacuo. The obtained residue was purified by chromatography (CH2Cl2:MeOH=50: l) resulting in an intermediate amide compound (50.6 g). Method A2; Rt: 1.15 min. m/z=:490.1 (M+Na)+ Exact mass: 467.1 A solution of the above obtained intermediate (50.61g), Na2C03 (34.5 lg. 325.6 mmol), H20 (300 mL) and CH3CH2OH (300 mL) was stirred for 3 hours at reflux. EtOH was removed in vacuo and the mixture was extracted with ethyl acetate (3 x 300 mL). The combined organic layers were dried over Na2S04 and concentrated in vacuo. The obtained residue was washed with t-butyl methyl ether resulting in compound QA-9 (39.2 g). Method A2; Rt: 1.37 min. m/z=:448.1 (M+H)+ Exact mass: 447.1
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