HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 906810-51-3
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 59772640 | HCID 59772640 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 906810-51-3 | HCID 66841763 | — |
Reaction Steps
A mixture of 1-Boc-2(S)-ethyl-4-benzyl-5(R)-methylpiperazine (A36; 13.6 g, 43 mmol), glacial acetic acid (2.5 mL) and 10% Pd/C (4.5 g) in methanol (150 mL) was shaken under H2 atmosphere (50 psi) for 24 h. The mixture was filtered through Celite® and the filter cake was washed copiously with EtOAc (˜500 mL). The combined filtrates were dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure to afford a clear colorless oil. Further co-evaporation with CH2Cl2 (200 mL) and Et2O (2×200 mL) gave the desired 1-Boc-2(S)-ethyl-5(R)-methylpiperazine acetic acid salt (A37, 9.7 g) as a viscous oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902199B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-93321ab9f2d24313a568f83c5555d912 |
| Source note | uspto-grants-2011_03 |