3-(methylsulfonimidoyl)aniline

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

実験手順: A solution of 200 mg (1.00 mmol) of (RS)—S-methyl-S-(3-nitrophenyl)sulfoximide in 20 ml of THF is mixed at room temperature with 8 ml of an approximately 10% solution of Ti(III)Cl in 20-30% hydrochloric acid. After 3 hours, another 2 ml of the approximately 10% solution of Ti(III)Cl in 20-30% hydrochloric acid is added and stirred overnight at room temperature. The batch is made basic with 1N NaOH solution and mixed with ethyl acetate. It is filtered, and the filter cakes are washed with ethyl acetate/MeOH (3:2). The organic solvent is drawn off in a rotary evaporator, and the residue is extracted from ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated by evaporation. The residue that is obtained is purified by chromatography (DCM/EtOH 95:5). 82 mg (0.48 mmol, corresponding to 48% of theory) of the product is obtained. It is filtered the filter cakes are washed with ethyl acetate/MeOH (3:2) The organic solvent is drawn off in a rotary evaporator the residue is extracted from ethyl acetate The combined organic phases are dried (Na2SO4) filtered concentrated by evaporation The residue that is obtained is purified by chromatography (DCM/EtOH 95:5) 82 mg (0.48 mmol, corresponding to 48% of theory) of the product is obtained

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

実験手順: 127 mg (0.43 mmol) of (R)-3-[(5-bromo-2-chloropyrimidin-4-yl)amino]-2-methyl-butan-2-ol in 1 ml of acetonitrile is added to 74 mg (0.43 mmol) of (RS)—S-(3-aminophenyl)-S-methyl sulfoximide in 0.5 ml of acetonitrile. It is mixed with 0.1 ml of a 4N solution of HCl in dioxane, and the batch is refluxed overnight. The solvent is drawn off, and the remaining residue is purified by chromatography (DCM/EtOH 9:1). 37 mg (0.09 mmol, corresponding to 20% of theory) of the product is obtained. the batch is refluxed overnight the remaining residue is purified by chromatography (DCM/EtOH 9:1) 37 mg (0.09 mmol, corresponding to 20% of theory) of the product is obtained

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

実験手順: A solution of 200 mg (1.00 mmol) of (RS)-S-methyl-S-(3-nitrophenyl)sulfoximide in 20 ml of THF is mixed at room temperature with 8 ml of an approximately 10% solution of Ti(III)Cl in 20-30% hydrochloric acid. After 3 hours, another 2 ml of the approximately 10% solution of Ti(III)Cl in 20-30% hydrochloric acid is added and stirred overnight at room temperature. The batch is made basic with 1N NaOH solution and mixed with ethyl acetate. It is filtered, and the filter cakes are washed with ethyl acetate/MeoH (3:2). The organic solvent is drawn off in a rotary evaporator, and the residue is extracted from ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated by evaporation. The residue that is obtained is purified by chromatography (DCM/EtOH 95:5). 0.82 mg (0.48 mmol, corresponding to 48% of theory) of the product is obtained. It is filtered the filter cakes are washed with ethyl acetate/MeoH (3:2) The organic solvent is drawn off in a rotary evaporator the residue is extracted from ethyl acetate The combined organic phases are dried (Na2SO4) filtered concentrated by evaporation The residue that is obtained is purified by chromatography (DCM/EtOH 95:5) 0.82 mg (0.48 mmol, corresponding to 48% of theory) of the product is obtained

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

実験手順: 127 mg (0.43 mmol) of (R)-3-[(5-bromo-2-chloropyrimidin-4-yl)amino]-2-methyl-butan-2-ol in 1 ml of acetonitrile is added to 74 mg (0.43 mmol) of (RS)-S-(3-aminophenyl)-S-methyl sulfoximide in 0.5 ml of acetonitrile. It is mixed with 0.1 ml of a 4N solution of HCl in dioxane, and the batch is refluxed overnight. The solvent is drawn off, and the remaining residue is purified by chromatography (DCM/EtOH 9: 1). 37 mg (0.09 mmol, corresponding to 20% of theory) of the product is obtained. the batch is refluxed overnight the remaining residue is purified by chromatography (DCM/EtOH 9: 1) 37 mg (0.09 mmol, corresponding to 20% of theory) of the product is obtained