HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → (2S)-2-(4-Methoxybutyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | (S)-2-(4-Methoxybutyl)-piperazine-1,4-dicarboxylic acid di-tert-butyl ester | HCID 58625892 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2S)-2-(4-Methoxybutyl)piperazine | HCID 45099588 | — |
Reaction Steps
Into a stirred, room temperature solution of (S)-2-(4-methoxybutyl)-piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.198 g, 0.53 mmol) in CH2Cl2 (2.6 mL), add TFA (2.6 mL) and stir for 2 h. Concentrate the mixture under reduced pressure, dilute with H2O and load onto an SCX column (10 g). Wash the resin with H2O (3×100 mL), MeOH (3×100 mL) and elute the product with 2 M NH3 in MeOH (3×100 mL). Concentrate the purified fractions under reduced pressure and azeotrope the residue with CH2Cl2/hexanes (1:2). Place the residue under vacuum to give the title compound: orange crystals (0.093 g), mass spectrum (m/e):173.4 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07384934B2 |
| Source dataset | uspto-grants-2008_06 |
| ORD ID | ord-7a0edb1d2f96414490800c2dca4d75ef |
| Source note | uspto-grants-2008_06 |