methyl 2-iodo-3-methoxybenzoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A stirred mixture of 2-iodo-3-methoxybenzoic acid (20 g, 0.07 mol; prepared in a manner similar to that described above), methanol (300 ml) and concentrated sulphuric acid (3.5 ml) was heated under reflux for 8 hours, cooled to ambient temperature and added to water (1500 ml). The product was extracted into dichloromethane (3×500 ml), the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml), then they were dried (MgSO4) and the solvent was removed in vacuo to give methyl 2-iodo-3-methoxybenzoate (18.5 g, 90%) as a solid, m.pt. 58–61° C. prepared in a manner similar to was heated under reflux for 8 hours The product was extracted into dichloromethane (3×500 ml) the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml) they were dried (MgSO4) the solvent was removed in vacuo

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

実験手順: Using the procedure outlined in Step A of Example 18, 201.7 mg (0.69 mmol) of methyl-2-iodo-3-methoxy-benzoate and 125.9 mg (0.82 mmol) of 2-methoxy-phenylboronic acid gave after 27 hours of reflux a quantitative yield of the title substance. gave after 27 hours of reflux a quantitative yield of the title substance

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

実験手順: A stirred mixture of 2-iodo-3-methoxybenzoic acid (20 g, 0.07 mol; prepared in a manner similar to that described above), methanol (300 ml) and concentrated sulphuric acid (3.5 ml) was heated under reflux for 8 hours, cooled to ambient temperature and added to water (1500 ml). The product was extracted into dichloromethane (3×500 ml), the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml), then they were dried (MgSO4) and the solvent was removed in vacuo to give methyl 2-iodo-3-methoxybenzoate (18.5 g, 90%) as a solid, m.pt. 58-61° C. prepared in a manner similar to was heated under reflux for 8 hours The product was extracted into dichloromethane (3×500 ml) the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml) they were dried (MgSO4) the solvent was removed in vacuo

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

実験手順: A stirred mixture of 2-iodo-3-methoxybenzoic acid (20 g, 0.07 mol; prepared in a manner similar to that described above), methanol (300 ml) and concentrated sulphuric acid (3.5 ml) was heated under reflux for 8 hours, cooled to ambient temperature and added to water (1500 ml). The product was extracted into dichloromethane (3×500 ml), the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml), then they were dried (MgSO4) and the solvent was removed in vacuo to give methyl 2-iodo-3-methoxybenzoate (18.5 g, 90%) as a solid, m.pt. 58-61° C. prepared in a manner similar to was heated under reflux for 8 hours The product was extracted into dichloromethane (3×500 ml) the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml) they were dried (MgSO4) the solvent was removed in vacuo

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

実験手順: Using the procedure outlined in Example 10, 201.7 mg (0.69 mmol) of methyl-2-iodo-3-methoxy-benzoate and 125.9 mg (0.82 mmol) of 2-methoxy-phenylboronic acid gave after 27 hours of reflux a quantitative yield of the title substance. gave after 27 hours of reflux a quantitative yield of the title substance

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

実験手順: A stirred mixture of 2-iodo-3-methoxybenzoic acid (20 g, 0.07 mol; prepared in a manner similar to that described above), methanol (300 ml) and concentrated sulphuric acid (3.5 ml) was heated under reflux for 8 hours, cooled to ambient temperature and added to water (1500 ml). The product was extracted into dichloromethane (3×500 ml), the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml), then they were dried (MgSO4) and the solvent was removed in vacuo to give methyl 2-iodo-3-methoxybenzoate (18.5 g, 90%) as a solid, m.pt. 58–61° C. prepared in a manner similar to was heated under reflux for 8 hours The product was extracted into dichloromethane (3×500 ml) the combined extracts were washed with 5% aqueous sodium hydroxide solution (3×500 ml) they were dried (MgSO4) the solvent was removed in vacuo

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

実験手順: Using the procedure outlined in Step A of Example 18, 201.7 mg (0.69 mmol) of methyl-2-iodo-3-methoxy-benzoate and 125.9 mg (0.82 mmol) of 2-methoxy-phenylboronic acid gave after 27 hours of reflux a quantitative yield of the title substance. gave after 27 hours of reflux a quantitative yield of the title substance