1-(2-chloroethyl)-3-methoxybenzene

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

実験手順: A mixture of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(methylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (1.07 g), methylene chloride (20 ml), 3-methoxyphenethyl chloride (500 mg), triethylamine (313 mg) and sodium iodide (30 mg) is stirred at room temperature for 48 hours. After the completion of the reaction, the solvent is distilled off, and the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1) to give (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-{2-[N-methyl-N-(3-methoxyphenethyl)amino]ethyl}-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (625 mg) as oily product. After the completion of the reaction the solvent is distilled off the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1)

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

実験手順: A mixture of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(methylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (1.07 g), methylene chloride (20 ml), 3-methoxyphenethyl chloride (500 mg), triethylamine (313 mg) and sodium iodide (30 mg) is stirred at room temperature for 48 hours. After the completion of the reaction, the solvent is distilled off, and the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1) to give (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-{2-[N-methyl-N-(3-methoxyphenethyl)amino]ethyl}-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (625 mg) as oily product. After the completion of the reaction the solvent is distilled off the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1)

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

実験手順: A mixture of 67 g of 1-(2-chloroethyl)-3-methoxybenzene, 53.1 g of 1H-imidazole, 99 g of sodium carbonate, 500 ml of 4-methyl-2-pentanone and a few crystals of potassium iodide was stirred for 48 hours at reflux temperature. After cooling, the reaction mixture was diluted with water and extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated and the residue was destilled (13.3 Pa; 160° C.), yielding 49.5 g (62.8%) of 1-[2-(3-methoxyphenyl)ethyl]-1H-imidazole (interm. 10). at reflux temperature After cooling extracted with 4-methyl-2-pentanone The extract was dried filtered evaporated (13.3 Pa; 160° C.)

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

実験手順: A mixture of 67 g of 1-(2-chloroethyl)-3-methoxybenzene, 53.1 g of 1H-imidazole, 99 g of sodium carbonate, 500 ml of 4-methyl-2-pentanone and a few crystals of potassium iodide was stirred for 48 hours at reflux temperature. After cooling, the reaction mixture was diluted with water and extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated and the residue was destilled (13.3 Pa; 160° C.), yielding 49.5 g (62.8%) of 1-[2-(3-methoxyphenyl)ethyl]-1H-imidazole (interm. 10). at reflux temperature After cooling extracted with 4-methyl-2-pentanone The extract was dried filtered evaporated (13.3 Pa; 160° C.)

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

実験手順: A mixture of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(methylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (1.07 g), methylene chloride (20 ml), 3-methoxyphenethyl chloride (500 mg), triethylamine (313 mg) and sodium iodide (30 mg) is stirred at room temperature for 48 hours. After the completion of the reaction, the solvent is distilled off, and the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1) to give (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-{2-[N-methyl-N-(3-methoxyphenethyl)amino]ethyl}-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (625 mg) as oily product. After the completion of the reaction the solvent is distilled off the resulting residue is purified by silica gel column chromatography (eluent; chloroform: ethanol=15:1)

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

実験手順: A mixture of 67 g of 1-(2-chloroethyl)-3-methoxybenzene, 53.1 g of 1H-imidazole, 99 g of sodium carbonate, 500 ml of 4-methyl-2-pentanone and a few crystals of potassium iodide was stirred for 48 hours at reflux temperature. After cooling, the reaction mixture was diluted with water and extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated and the residue was destilled (13.3 Pa; 160° C.), yielding 49.5 g (62.8%) of 1-[2-(3-methoxyphenyl)ethyl]-1H-imidazole (interm. 10). at reflux temperature After cooling extracted with 4-methyl-2-pentanone The extract was dried filtered evaporated (13.3 Pa; 160° C.)