HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 86710155, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Iodo-3-methylbutane | HCID 10924 | — |
| Reactant | HCID 69672723 | HCID 69672723 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86710155 | HCID 86710155 | 44% |
Reaction Steps
A suspension of Example 17F (814 mg, 3.83 mmol) and cesium carbonate (1.87 g, 5.75 mmol) in N,N-dimethylformamide was treated with isoamyl iodide (555 μL, 835 mg, 4.22 mmol) followed by stirring at room temperature for 48 hours. The mixture was diluted with ethyl acetate and extracted with water (3×) and saturated sodium chloride solution. Drying (Na2SO4) and concentration in vacuo afforded an amber oil, which was chromatographed over a 50 g silica gel cartridge, eluting with 15-70% ethyl acetate in dichloromethane. These procedures afforded the product (474 mg, 44%) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09173887B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-a9eb889d7d8a46b0aa43dfe671e0c9ab |
| Source note | uspto-grants-2015_11 |