ethyl 2-amino-5-bromobenzoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Amino-5-bromobenzoic acid (24.7 g, 11.4 mol) was dissolved in 350 mL of ethanol and 2, and 5 mL of concentrated H2SO4 was added. The mixture was refluxed under N2 for 12 h. The solvent was removed and the residue was added with EtOAc. The mixture was extracted with 1N NaOH. The organic solution was washed with brine, dried over MgSO4. It was concentrated and chromatographed with CH2Cl2 to give 3.19 g of 2-amino-5-bromobenzoic acid, ethyl ester. MS (AP+): 243.9, 246, M+H. The mixture was refluxed under N2 for 12 h The solvent was removed the residue was added with EtOAc The mixture was extracted with 1N NaOH The organic solution was washed with brine dried over MgSO4 It was concentrated chromatographed with CH2Cl2

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: As in scheme 1 step 1, from 2-amino-5-bromobenzoic acid, ethanol and HCl gas and heating under reflux for 16 h to afford an off-white solid, mp 83° C. under reflux for 16 h to afford an off-white solid, mp 83° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Amino-5-bromobenzoic acid (24.7 g, 11.4 mol) was dissolved in 350 mL of ethanol and 2, and 5 mL of concentrated H2SO4 was added. The mixture was refluxed under N2 for 12 h. The solvent was removed and the residue was added with EtOAc. The mixture was extracted with 1N NaOH. The organic solution was washed with brine, dried over MgSO4. It was concentrated and chromatographed with CH2Cl2 to give 3.19 g of 2-amino-5-bromobenzoic acid, ethyl ester. MS (AP+): 243.9, 246, M+H. The mixture was refluxed under N2 for 12 h The solvent was removed the residue was added with EtOAc The mixture was extracted with 1N NaOH The organic solution was washed with brine dried over MgSO4 It was concentrated chromatographed with CH2Cl2