3-chloropropylsulfanylbenzene

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:

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:

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:

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

実験手順: The title compound is prepared from N-[3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-propyl]-methylamine and 3-phenylthiopropylchloride analogously to Example 3. M.p. of the hydrochloride: 130°-140° C. 130°-140° C.

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

実験手順: A mixture of 8.30 g (44.5 mmols) of 1-chloro-3-phenylthiopropane, 100 ml of diethanolamine, 13.3 g (88.7 mmols) of sodium iodide and 250 ml of dioxan was heated under reflux for 15 hours. The mixture was concentrated under reduced pressure, and an aqueous saturated sodium bicarbonate solution was added to the mixture followed by extraction of the solution with chloroform 5 times. The chloroform layer was drided over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: chloroform/methanol =25/1) to afford 6.46 g (yield: 57%) of 1-bis(hydroxyethyl)amino-3-phenylthiopropane. was heated under reflux for 15 hours The mixture was concentrated under reduced pressure an aqueous saturated sodium bicarbonate solution was added to the mixture followed by extraction of the solution with chloroform 5 times The solvent was evaporated under reduced pressure the residue was purified by silica gel column chromatography (eluent: chloroform/methanol =25/1)

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

実験手順: A mixture of 54.0 g (490 mmols) of thiophenol, 160.0 g (1016 mmols) of 1-bromo-3-chloropropane and 250 ml of a 2.2 M aqueous sodium hydroxide solution was heated under reflux for 30 hours. After cooling, the reaction mixture was extracted with methylene chloride. The methylene chloride layer was washed with an aqueous dil. sodium hydroxide solution and then with water and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was distilled under reduced pressure (138 -140° C./13 mmHg) to afford 51.9 g (yield: 57%) of the title compound. was heated under reflux for 30 hours After cooling the reaction mixture was extracted with methylene chloride The methylene chloride layer was washed with an aqueous dil. sodium hydroxide solution with water and dried over anhydrous sodium sulfate The solvent was evaporated under reduced pressure the residue was distilled under reduced pressure (138 -140° C./13 mmHg)