HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 3-[4-(tert-Butoxycarbonyl)piperazin-1-yl]-3-oxopropionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | 3-[4-(tert-Butoxycarbonyl)piperazin-1-yl]-3-oxopropionic acid methyl ester | HCID 20622412 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[4-(tert-Butoxycarbonyl)piperazin-1-yl]-3-oxopropionic acid | HCID 23435445 | — |
Reaction Steps
3-[4-(tert-Butoxycarbonyl)piperazin-1-yl]-3-oxopropionic acid methyl ester (35) (3.30 g; 11.5 mmol) is dissolved in 2:2:2 tetrahydrofuran: water: methanol. Lithium chloride (2.76 g; 115.3 mmol) is added and the mixture is stirred for 1 hour at ambient temperature. The solution is concentrated in vacuo to remove the tetrahydrofuran and methanol. The concentrate is poured onto citric acid solution (115 mL) and extracted with ethyl acetate (230 mL). The organic layer is washed with water (3×115 mL) and brine (1×115 mL), then dried over magnesium sulfate, filtered and concentrated in vacuo to afford the desired product as a solid. ESMS: MH+ 273.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07304053B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-4ecd6495e1a64be892ef9bd0475df29e |
| Source note | uspto-grants-2007_12 |