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温度

0 °C

A solution of aminoacetaldehyde dimethyl acetal (25 mL, 229 mmol) in toluene (120 mL) is treated at 0° C. with a 4.85 M sodium hydroxide solution (70.8 mL, 343.5 mmol). The mixture is stirred at 0° C. for 10 minutes and benzyl chloroformate (33.8 mL, 229 mmol) is added keeping the internal temperature below 20° C. during the addition. The mixture is warmed to room temperature over 4 hours. The organic layer is separated, washed with brine, dried over sodium sulfate, and concentrated to dryness to give the title compound (54 g, 98%). ES/MS (m/e): 240 (M+H).

1. customthe internal temperature below 20° C.
2. additionduring the addition
3. temperatureThe mixture is warmed to room temperature over 4 hours
4. customThe organic layer is separated
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated to dryness