HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 2-[4-(4-Bromo-phenyl)piperazine-1-sulfonylmethyl]3-methylbutyric acid tert-butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-(4-Bromophenyl)piperazine hydrochloride | HCID 14422838 | — |
| Edukt | 2-Chlorosulfonylmethyl-3-methyl-butyric acid tert-butyl ester | HCID 21259094 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-[4-(4-Bromo-phenyl)piperazine-1-sulfonylmethyl]3-methylbutyric acid tert-butyl ester | HCID 69895250 | 79% |
Reaktionsschritte
A stirred suspension of 4-bromophenylpiperazine hydrochloride (2.84 g) and 2-chlorosulfonylmethyl-3-methyl-butyric acid tert-butyl ester (2.77 g) [preparation described in WO-A-98/05635] in dichloromethane (50 ml), cooled in an ice-bath, was treated with triethylamine (2 99 ml). The reaction was then stirred at room temperature for 2 h. The reaction mixture was then evaporated in vacuo, and the residue was dissolved in ethyl acetate (75 ml) and washed with 1% aqueous citric acid (2×50 ml), water (50 ml), saturated sodium bicarbonate (50 ml), saturated brine (50 ml), dried (MgSO4) and concentrated in vacuo to provide the title compound as a pale yellow gum (3.81 g, 79%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06809100B2 |
| Quelldatensatz | uspto-grants-2004_10 |
| ORD ID | ord-a8811c805f3a4f718c2c27961760b7a6 |
| Quellennotiz | uspto-grants-2004_10 |