HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 178472857, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86662102 | HCID 86662102 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178472857 | HCID 178472857 | — |
Reaction Steps
Ethyl 3-(3-chloro-2-thienyl)-2-diazo-3-oxopropanoate (662 mg, 2.56 mmol) was dissolved in dioxane (10 mL), treated with tri-n-butylphosphine (0.663 mL, 2.69 mmol, 1.05 equiv) and stirred at ambient temperature for 30 minutes. The mixture was poured into sodium bicarbonate (100 mL, aqueous saturated) and extracted with ethyl acetate (3×100 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 1:1; hexanes:ethyl acetate), providing the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08293744B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-601e5204adc6438691679eac9adec9f9 |
| Source note | uspto-grants-2012_10 |