[2-chloroethoxy(phenyl)methyl]benzene

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:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3.27 g of 2-chloroethanol in dry benzene (3.5 ml) was added 0.8 g of conc. sulfuric acid and the mixture was heated, under argon atmosphere, at 50° C. To the mixture was added slowly a solution of 5.0 g of benzhydrol in dry benzene (6.5 ml) and, after 30 minutes from the addition, the whole mixture was refluxed for 1.5 hours. After the mixture was allowed to cool, the benzene layer was washed with water and dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure, to give 6.7 g of benzhydryl 2-chloroethyl ether. after 30 minutes from the addition the whole mixture was refluxed for 1.5 hours to cool the benzene layer was washed with water dried over anhydrous sodium sulfate The solvent was removed by distillation under reduced pressure

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

実験手順: Following a procedure similar to that described in Preparation 1, but using 2-(diphenylmethoxy)ethyl chloride and homopiperazine, the title compound was obtained ina yield of 68%. that described in Preparation 1

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

実験手順: Following a procedure similar to that described in Preparation 5(c), but using 2-(diphenylmethoxy)ethyl chloride and anhydrous piperazine, the title compound was obtained in a yield of 75%.

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

実験手順: A mixture of 3 g (12.2 mmole) of 2- (diphenyl-methoxy)ethyl chloride, 5 g (49 mmole) of N,N' -dimethyl-propanediamine and 40 ml of toluene was heated under reflux overnight. At the end of this time, the toluene layer was separated and washed with water; 25 ml of a 10% w/v aqueous solution of acetic acid was then added thereto. The aqueous layer was separated, and a 10% w/v aqueous solution of sodium hydroxide was added to make it alkaline. The mixture was then extracted with diethyl ether, and the solvent was removed by distillation under reuced pressure, to obtain 2.4 g (yield 63%) of the title compound as an oil. was heated under reflux overnight At the end of this time, the toluene layer was separated washed with water 25 ml of a 10% w/v aqueous solution of acetic acid was then added The aqueous layer was separated a 10% w/v aqueous solution of sodium hydroxide was added The mixture was then extracted with diethyl ether the solvent was removed by distillation under reuced pressure

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: Following a procedure similar to that described in Preparation 1, but using 2-(diphenylmethoxy)ethyl chloride and homopiperazine, the title compound was obtained ina yield of 68%. that described in Preparation 1

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

実験手順: Following a procedure similar to that described in Preparation 5(c), but using 2-(diphenylmethoxy)ethyl chloride and anhydrous piperazine, the title compound was obtained in a yield of 75%.

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

実験手順: A mixture of 3 g (12.2 mmole) of 2- (diphenyl-methoxy)ethyl chloride, 5 g (49 mmole) of N,N' -dimethyl-propanediamine and 40 ml of toluene was heated under reflux overnight. At the end of this time, the toluene layer was separated and washed with water; 25 ml of a 10% w/v aqueous solution of acetic acid was then added thereto. The aqueous layer was separated, and a 10% w/v aqueous solution of sodium hydroxide was added to make it alkaline. The mixture was then extracted with diethyl ether, and the solvent was removed by distillation under reuced pressure, to obtain 2.4 g (yield 63%) of the title compound as an oil. was heated under reflux overnight At the end of this time, the toluene layer was separated washed with water 25 ml of a 10% w/v aqueous solution of acetic acid was then added The aqueous layer was separated a 10% w/v aqueous solution of sodium hydroxide was added The mixture was then extracted with diethyl ether the solvent was removed by distillation under reuced pressure

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 (2'-diphenylmethoxyethyl)-oxyamine hydrochloride is prepared from 1-chloro-2-(diphenylmethoxy)-ethane in an analogous fashion to that described in Example 10 for p-fluorobenzyloxyamine hydrochloride.