HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 67273555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | tert-Butyl(2-iodoethoxy)dimethylsilane | HCID 11129873 | — |
| Reactant | 4-Methylsulfanyl-pyridine-2,6-diamine | HCID 67274504 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67273555 | HCID 67273555 | 22% |
Reaction Steps
In a glass vessel were mixed together the above prepared 4-methylsulfanyl-pyridine-2,6-diamine (0.350 g, 2.25 mmol), tert-butyl-(2-iodo-ethoxy)-dimethyl-silane (CAS 101166-65-8, 0.700 g, 1.08 eq.), and 1.2 eq. of Cs2CO3 (0.882 g) in 3.5 mL of abs. acetonitrile, and the mixture allowed to react for 2 h at 125° C. in a microwave oven. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=4/6) afforded 0.155 g of the title compound as light brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163778B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-c4ae1a5242ec4ad880edf42c07071d8a |
| Source note | uspto-grants-2012_04 |