反应详情

1,4-Dioxa-8-azaspiro[4.5]decane (1.76 g), 2-chloro-5-ethylpyrimidine (1.7 g), N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (5.07 ml) are heated in a sealed vessel at 120° C. with stirring for 22 h. After cooling the mixture is concentrated and partitioned between ethyl acetate (100 mL) and water (100 mL). The water layer is extracted with ethyl acetate (100 mL) and the combined ethyl acetate layers are dried over Na2SO4, filtered and concentrated to give the title compound. LC (method 20): tR=1.73 min; Mass spectrum (APCI): m/z=250 [M+H]+.

1. temperatureAfter cooling the mixture
2. concentrationis concentrated
3. custompartitioned between ethyl acetate (100 mL) and water (100 mL)
4. extractionThe water layer is extracted with ethyl acetate (100 mL)
5. dry with materialthe combined ethyl acetate layers are dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated