HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 8-t-Butyl-2-(4,6-dimethoxy pyrimid-2-ylaminomethyl)-1,4-dioxaspiro(4,5)decane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4,6-Dimethoxy-2-(methylsulfonyl)pyrimidine | HCID 838363 | — |
| Reactant | 8-t-Butyl-2-aminomethyl-1,4-dioxaspiro(4,5)decane | HCID 19963665 | — |
| Product | 8-t-Butyl-2-(4,6-dimethoxy pyrimid-2-ylaminomethyl)-1,4-dioxaspiro(4,5)decane | HCID 19963663 | 66% |
Reaction Steps
8-t-butyl-2-aminomethyl-1,4-dioxaspiro(4,5)decane (3.3 g, 14.5 mmol), 4,6-dimethoxy-2-methylsulfonyl-pyrimidine (3.16 g, 14.5 mmol) and potassium carbonate (2.76 g, 20 mmol) were heated to 160° C. for 1 hour. The reaction mixture was then extracted with toluene and the concentrated extracts purified by flash chromatography using a 3:1 mixture of toluene and ethylacetate. 3.5 g of a faint yellow oil was obtained which crystallised on standing. NMR analysis indicated the product being a mixture of diastereoisomers. M.p.: 76°-106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05616708 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-bf70ebbb219e42a3a411d90380f15213 |
| Source note | uspto-grants-1997_04 |