ethyl 3-methyl-3-(methylamino)butanoate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture containing ethyl 3-methyl-3-methylaminobutanoate (95 g-see Preparation 8), benzyl bromide (72 ml), anhydrous potassium carbonate (138 g) and acetonitrile (500 ml) was heated under reflux for 1.5 hours. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml). The layers were separated and the aqueous layer extracted with dichloromethane (2×100 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give the title compound as a mobile, colourless oil, yield 150 g. was heated under reflux for 1.5 hours The mixture was concentrated in vacuo the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml) The layers were separated the aqueous layer extracted with dichloromethane (2×100 ml) The combined dichloromethane extracts were dried (MgSO4) concentrated in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture containing ethyl 3-methyl-3-methylaminobutanoate (95 g--see Preparation δ), benzyl bromide (72 ml), anhydrous potassium carbonate (138 g) and acetonitrile (500 ml) was heated under reflux for 1.5 hours. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml). The layers were separated and the aqueous layer extracted with dichloromethane (2×100 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give the title compound as a mobile, colourless oil, yield 150 g. was heated under reflux for 1.5 hours The mixture was concentrated in vacuo the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml) The layers were separated the aqueous layer extracted with dichloromethane (2×100 ml) The combined dichloromethane extracts were dried (MgSO4) concentrated in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture containing ethyl 3-methyl-3-methylaminobutanoate (95 g--Preparation 5), benzyl bromide (72 ml), anhydrous potassium carbonate (138 g) and acetonitrile (500 ml) was heated under reflux for 1.5 hours. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml). The layers were separated and the aqueous layer extracted with dichloromethane (2 ×100 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give an the title compound as a mobile, colourless oil, yield, 150 g. was heated under reflux for 1.5 hours The mixture was concentrated in vacuo the residue partitioned between dichloromethane (500 ml) and 10% aqueous potassium carbonate (300 ml) The layers were separated the aqueous layer extracted with dichloromethane (2 ×100 ml) The combined dichloromethane extracts were dried (MgSO4) concentrated in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture containing ethyl 3,3-dimethylacrylate (100 g) and methylamine (140 ml of a 33% solution in ethanol) in ethanol (400 ml) was allowed to stand at room temperature for 2 weeks. The mixture was concentrated in vacuo to give an oil which was fractionally distilled in vacuo to give the title compound as a colourless, mobile oil, yield, 95.0 g, b.p. 68°-75°/20 mm.Hg. to stand at room temperature for 2 weeks The mixture was concentrated in vacuo to give an oil which was fractionally distilled in vacuo