HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 8-(5-Ethylpyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| Reactant | 2-Chloro-5-ethylpyrimidine | HCID 3572763 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 8-(5-Ethylpyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane | HCID 68290246 | — |
Reaction Steps
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]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921398B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-df9cad120e514d46ba0785ad589c5d01 |
| Source note | uspto-grants-2014_12 |