2-amino-2-methylpentanenitrile

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

実験手順: 64.21 g (294.18 mmol) of di-tert-butyl dicarbonate were initially charged in a round-bottom flask, and 30 g (267.44 mmol) of rac-2-amino-2-methylpentanenitrile were added very gradually at RT (internal thermometer, maximum temperature 30° C.), and stirring of the mixture was continued at room temperature overnight. The reaction mixture was admixed with dichloromethane and washed twice with 1 N sodium hydroxide solution. The organic phase was dried over sodium sulphate, filtered and concentrated (at bath temperature 30° C.). 76.33 g (quantitative yield) of the target compound were obtained. washed twice with 1 N sodium hydroxide solution The organic phase was dried over sodium sulphate filtered concentrated (at bath temperature 30° C.)

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

実験手順: 20 g (178.3 mmol) of rac-2-amino-2-methylpentanonitrile (described in: Deng, S L. et al., Synthesis 2001, 2445-2449; Freifelder, M. et al., J. Am. Chem. Soc. 1960, 696-698) were initially charged in 2.63 l of THF/water (8/1), and 76.4 g (552.7 mmol) of potassium carbonate were added. Then 27.6 ml (196.1 mmol) of benzyl chloroformate were slowly added dropwise at 0° C. and the mixture was stirred at RT overnight. The reaction mixture was concentrated, and the residue was admixed with water and extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue was purified by means of silica gel chromatography (eluent:cyclohexane/ethyl acetate=4/1). 43.84 g of the target compound were obtained (76% of theory, 76% purity). The reaction mixture was concentrated extracted twice with ethyl acetate The combined organic phases were dried over sodium sulphate filtered concentrated The residue was purified by means of silica gel chromatography (eluent:cyclohexane/ethyl acetate=4/1)