HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 57478572, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl ketone | HCID 7288 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57478572 | HCID 57478572 | 68.9% |
Reaction Steps
A mixture of piperazine-1-carboxylic acid tert-butyl ester (7.00 g), 3-pentanone (3.89 g), glacial acetic acid (2.22 mL) and sodium triacetoxyborohydride (11.95 g) in dichloromethane (DCM, 200 mL) was stirred for 18 h at room temperature. The reaction mixture was quenched with 1 N aqueous NaOH (80 mL) and stirred for 2.5 h at room temperature. Additional water (100 mL) was added, and the resulting mixture was extracted with DCM (3×100 mL). Extracts were combined and washed with water (2×100 mL), dried (Na2SO4), and concentrated under reduced pressure, yielding the title compound (6.28 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07414047B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-4d354cd536034b1589bd26c0caba6fdf |
| Source note | uspto-grants-2008_08 |