HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → tert-Butyl 4-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrile | HCID 93865 | — |
| Reactant | Ethyl piperazine-1-acetate | HCID 207112 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | tert-Butyl 4-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate | HCID 22321826 | — |
Reaction Steps
1-(Ethoxycarbonylmethyl)-piperazine (5.00 g, 29.0 mmol) is dissolved in 35 mL of 50% aqueous dioxane. Triethylamine (4.41 g, 43.5 mmol) is added followed by 2-(tert-butoxycarbonyloxyimino)-2-phenylacetonitrile (7.86 g, 31.9 mmol). The reaction is stirred for 14.5 hours at ambient temperature, then poured onto water and extracted with ethyl acetate (2×100 mL). The combined organic extracts are washed with water (3×100 mL), brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue is purified via silica gel chromatography with gradient elution (20%→50% ethyl acetate in hexanes) affording the desired product as an oil. CIMS: MH+ 273.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07304053B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-7b99892e29ba402d8d16fc8fad62aaa3 |
| Source note | uspto-grants-2007_12 |