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温度

0 °C

To a solution of 1,4-dioxa-8-azaspiro[4,5]decane (9.80 g, 67.1 mmol) in dichloromethane (150 mL) under nitrogen was added triethylamine (11.2 mL, 80.5 mmol. This was then cooled to 0° C. and to this was added dropwise with stirring 2-chloroacetyl chloride (6.53 mL, 80.5 mmol) in dichloromethane (50 mL) over 1 and a half hours. This was then stirred overnight warming to room temperature in the process. The reaction was then quenched by adding 1 N HCl (100 mL). This was then extracted with ethyl acetate and the ethyl acetate layers were dried with solid anhydrous magnesium sulfate powder, filtered and concentrated to give 2-Chloro-1-(1,4-dioxa-8-azaspiro[4,5]decan-8-yl)ethan-1-one as a brown oil (15.44 g). This was used without purification for the next step.

1. temperaturewarming to room temperature in the process
2. customThe reaction was then quenched
3. additionby adding 1 N HCl (100 mL)
4. extractionThis was then extracted with ethyl acetate
5. dry with materialthe ethyl acetate layers were dried with solid anhydrous magnesium sulfate powder
6. filtrationfiltered
7. concentrationconcentrated