HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trifluoroacetic acid → 1-(3-Chlorobenzyl)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | Tert-butyl 4-[(3-chlorophenyl)methyl]piperazine-1-carboxylate | HCID 4316940 | — |
| Produkt | 1-(3-Chlorobenzyl)piperazine | HCID 764727 | — |
Reaktionsschritte
To 4-(3-chlorobenzyl)-piperazine-1-carboxylic acid tert-butyl ester (20.24) (8.82 g, 28.4 mmol) is added TFA (45 mL) at ambient temperature over 5 min. After 1 h 50 min, TFA is evaporated, the residue is dissolved in 2N HCl (45 mL) and extracted with ether (2×45 mL). The aqueous layer is basified to pH 13 with 2N NaOH (60 mL) and extracted with CH2Cl2 (6×90 mL). The combined organic extracts are washed with brine (75 mL) and dried over MgSO4. The crude material obtained after filtration and concentration (5.44 g, 25.8 mmol, 91%) is used without further purification. MS (ES): m/z 211.0/213.0 (100/35) [MH+]. tR (method B)=5.1 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07501407B2 |
| Quelldatensatz | uspto-grants-2009_03 |
| ORD ID | ord-d33f0fe59b9f4c7fb9bb1a4030d09d4b |
| Quellennotiz | uspto-grants-2009_03 |