HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxaspiro[4.5]decan-8-one → 8-Pyrimidin-2-yl-1,4-dioxa-spiro[4.5]decan-8-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| Reactant | 2-Stannyl pyrimidine | HCID 87150656 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 8-Pyrimidin-2-yl-1,4-dioxa-spiro[4.5]decan-8-ol | HCID 59017433 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
To a solution of 2-stannyl pyrimidine (200 mmol, 80 g), prepared as previously described in the literature (Tetrahedron, 1994, 50, 275-284), in THF (1 L) was added n-butyllithium (240 mmol, 150 mL) at −78° C. The reaction was stirred for 30 min at −78° C. and 1,4-dioxa-spiro[4.5]decan-8-one (200 mmol, 30 g) was added. The reaction was allowed to stir overnight while warming to ambient temperature. The reaction was then quenched using NH4Cl and extracted using EtOAc (3×400 mL). The organic layers were combined and dried over MgSO4 and concentrated in vacuo. The crude was taken to the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834021B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-b6ceb8cd83c74973a52197b11088a518 |
| Source note | uspto-grants-2010_11 |