(4-BroMo-2-chlorophenyl)MethanaMine hydrochloride

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

実験手順: 46.2 ml of borane-THF complex are provided under ice cooling. A solution of 2.0 g of 4-bromo-4-chlorobenzonitrile in 240 ml of THF is added slowly. The reaction mixture is then heated for 1 h under reflux, cooled and 20 ml of 1N hydrochloric acid are added dropwise while cooling on ice. The mixture is heated under reflux for 1 h and left to cool. For the work-up the solution is adjusted to an alkaline pH with a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. 6 ml of hydrochloric acid in dioxane (4N) are added and the precipitated hydrochloride is collected by suction filtration. 1.3 g of product are obtained. 46.2 ml of borane-THF complex are provided under ice cooling The reaction mixture is then heated for 1 h under reflux cooled while cooling on ice The mixture is heated under reflux for 1 h left to cool extracted with dichloromethane The organic phase is dried over sodium sulfate concentrated on a rotary evaporator 6 ml of hydrochloric acid in dioxane (4N) are added the precipitated hydrochloride is collected by suction filtration

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

実験手順: 46.2 ml of borane-THF complex are provided under ice cooling. A solution of 2.0 g of 4-bromo-4-chlorobenzonitrile in 240 ml of THF is added slowly. The reaction mixture is then heated for 1 h under reflux, cooled and 20 ml of 1N hydrochloric acid are added dropwise while cooling on ice. The mixture is heated under reflux for 1 h and left to cool. For the work-up the solution is adjusted to an alkaline pH with a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. 6 ml of hydrochloric acid in dioxane (4N) are added and the precipitated hydrochloride is collected by suction filtration. 1.3 g of product are obtained. 46.2 ml of borane-THF complex are provided under ice cooling The reaction mixture is then heated for 1 h under reflux cooled while cooling on ice The mixture is heated under reflux for 1 h left to cool extracted with dichloromethane The organic phase is dried over sodium sulfate concentrated on a rotary evaporator 6 ml of hydrochloric acid in dioxane (4N) are added the precipitated hydrochloride is collected by suction filtration

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

実験手順: 46.2 ml of borane-THF complex are provided under ice cooling. A solution of 2.0 g of 4-bromo-4-chlorobenzonitrile in 240 ml of THF is added slowly. The reaction mixture is then heated for 1 h under reflux, cooled and 20 ml of 1N hydrochloric acid are added dropwise while cooling on ice. The mixture is heated under reflux for 1 h and left to cool. For the work-up the solution is adjusted to an alkaline pH with a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. 6 ml of hydrochloric acid in dioxane (4N) are added and the precipitated hydrochloride is collected by suction filtration. 1.3 g of product are obtained. 46.2 ml of borane-THF complex are provided under ice cooling The reaction mixture is then heated for 1 h under reflux cooled while cooling on ice The mixture is heated under reflux for 1 h left to cool extracted with dichloromethane The organic phase is dried over sodium sulfate concentrated on a rotary evaporator 6 ml of hydrochloric acid in dioxane (4N) are added the precipitated hydrochloride is collected by suction filtration

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

実験手順: 46.2 ml of borane-THF complex are provided under ice cooling. A solution of 2.0 g of 4-bromo-4-chlorobenzonitrile in 240 ml of THF is added slowly. The reaction mixture is then heated for 1 h under reflux, cooled and 20 ml of 1N hydrochloric acid are added dropwise while cooling on ice. The mixture is heated under reflux for 1 h and left to cool. For the work-up the solution is adjusted to an alkaline pH with a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. 6 ml of hydrochloric acid in dioxane (4N) are added and the precipitated hydrochloride is collected by suction filtration. 1.3 g of product are obtained. 46.2 ml of borane-THF complex are provided under ice cooling The reaction mixture is then heated for 1 h under reflux cooled while cooling on ice The mixture is heated under reflux for 1 h left to cool extracted with dichloromethane The organic phase is dried over sodium sulfate concentrated on a rotary evaporator 6 ml of hydrochloric acid in dioxane (4N) are added the precipitated hydrochloride is collected by suction filtration