methyl 2-amino-4,4-dimethylpentanoate

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: 2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1 The reaction mixture was concentrated in vacuo A white precipitate formed was filtered washed with EtOAc washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine The organic layer was dried over Na2SO4 decanted concentrated to a white solid (6.33 g)

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid (1.00 g, 6.84 mmol) was suspended in 50 mL of methanol and cooled in an ice bath. Thionyl chloride (1.82 g, 15.0 mmol) was added dropwise, at which time all the acid went into solution. The reaction was then removed from the ice bath and heated to reflux for 3.5 h. The reaction mixture was concentrated in vacuo and the resulting solid (1.10 g) was used in the next step without further purification. MS, m/z 159.9=M+1 cooled in an ice bath The reaction was then removed from the ice bath heated to reflux for 3.5 h The reaction mixture was concentrated in vacuo the resulting solid (1.10 g) was used in the next step without further purification

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1. The reaction mixture was concentrated in vacuo A white precipitate formed was filtered washed with EtOAc washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine The organic layer was dried over Na2SO4 decanted concentrated to a white solid (6.33 g)

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1. The reaction mixture was concentrated in vacuo A white precipitate formed was filtered washed with EtOAc washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine The organic layer was dried over Na2SO4 decanted concentrated to a white solid (6.33 g)

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid (1.00 g, 6.84 mmol) was suspended in 50 mL of methanol and cooled in an ice bath. Thionyl chloride (1.82 g, 15.0 mmol) was added dropwise, at which time all the acid went into solution. The reaction was then removed from the ice bath and heated to reflux for 3.5 h. The reaction mixture was concentrated in vacuo and the resulting solid (1.10 g) was used in the next step without further purification. MS, m/z 159.9=M+1. cooled in an ice bath The reaction was then removed from the ice bath heated to reflux for 3.5 h The reaction mixture was concentrated in vacuo the resulting solid (1.10 g) was used in the next step without further purification

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1 The reaction mixture was concentrated in vacuo A white precipitate formed was filtered washed with EtOAc washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine The organic layer was dried over Na2SO4 decanted concentrated to a white solid (6.33 g)

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid (1.00 g, 6.84 mmol) was suspended in 50 mL of methanol and cooled in an ice bath. Thionyl chloride (1.82 g, 15.0 mmol) was added dropwise, at which time all the acid went into solution. The reaction was then removed from the ice bath and heated to reflux for 3.5 h. The reaction mixture was concentrated in vacuo and the resulting solid (1.10 g) was used in the next step without further purification. MS, m/z 159.9=M+1 cooled in an ice bath The reaction was then removed from the ice bath heated to reflux for 3.5 h The reaction mixture was concentrated in vacuo the resulting solid (1.10 g) was used in the next step without further purification

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

実験手順: 2-Amino-4,4-dimethyl-pentanoic acid (1.00 g, 6.84 mmol) was suspended in 50 mL of methanol and cooled in an ice bath. Thionyl chloride (1.82 g, 15.0 mmol) was added dropwise, at which time all the acid went into solution. The reaction was then removed from the ice bath and heated to reflux for 3.5 h. The reaction mixture was concentrated in vacuo and the resulting solid (1.10 g) was used in the next step without further purification. MS, m/z 159.9=M+1 cooled in an ice bath The reaction was then removed from the ice bath heated to reflux for 3.5 h The reaction mixture was concentrated in vacuo the resulting solid (1.10 g) was used in the next step without further purification

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir: