HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium iodide → HCID 67954869, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium iodide | HCID 66321 | — |
| Reactant | HCID 67954671 | HCID 67954671 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67954869 | HCID 67954869 | 45% |
Reaction Steps
Ethyl 1-cyclohexyl-1,6-dihydro-6-oxo-2-phenyl-5-pyrimidinecarboxylate (1.41 g, 4.32 mmol) (i.e. the product from Example 11, Step A) was dissolved in ethyl acetate and treated with lithium iodide (powder, 1.72 g, 12.8 mmol) and heated to reflux for 16 h. The crude reaction mixture was concentrated under reduced pressure and then aqueous sodium bicarbonate was added and the resulting solution was extracted with ethyl acetate which was then discarded. The aqueous layer was made acidic with hydrochloric acid (1 N) and then extracted with dichloromethane (2×40 mL). The combined organic extracts were dried over MgSO4 and concentrated under reduced pressure resulting in 0.58 g of the title product as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952024B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-f5a05af909014f26b05acaac2ba3d023 |
| Source note | uspto-grants-2015_02 |