反应详情

To a solution of N,O-dimethylhydroxylamine hydrochloride (10 g, 102.52 mmol) and ethyl chlorooxoacetate (13.77 ml, 123.02 mmol) in dichloromethane (163 ml) at 0° C. was added triethylamine (28.6 ml, 205.04 mmol) drop wise. The reaction was stirred at room temperature for 1.5 hrs. The reaction was quenched with 20 ml of methanol, and then concentrated. The resulting solid was triturated with THF and filtered away. The filtrate was concentrated. The residue was vacuum distilled bulb to bulb. At approximately 85° C. impurities were collected and then discarded. The title compound was collected at approximately 120° C. as a neat oil (11.6 g, 72.0 mmol, 70.2%).

1. customThe reaction was quenched with 20 ml of methanol
2. concentrationconcentrated
3. customThe resulting solid was triturated with THF
4. filtrationfiltered away
5. concentrationThe filtrate was concentrated
6. distillationdistilled bulb to bulb
7. customAt approximately 85° C. impurities were collected