HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → 1-(3-Methanesulfonyl-benzoyl)-piperidin-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 3-Methanesulfonylbenzoic acid | HCID 220380 | — |
| Edukt | PyBroP | HCID 2733179 | — |
| Edukt | 4-Piperidone hydrochloride | HCID 3084851 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(3-Methanesulfonyl-benzoyl)-piperidin-4-one | HCID 22397490 | 93% |
Reaktionsschritte
PyBrOP™ (17.3 g) was added to a stirred mixture of 3-methanesulphonyl benzoic acid (7.35 g), 4-piperidone hydrochloride (5 g) and Hunig's base (25 ml) in dichloromethane (250 ml) with stirring at RT. The mixture was stirred overnight then washed with saturated NaHCO3 solution (200 ml) and then with saturated brine (200 ml). The organic layer was evaporated and the resulting residue purified by column chromatography (silica, 1:1 ethyl acetate: dichloromethane) to give the product as a thick oil (9.6 g; MS: APCI+(M+H) 282).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07238811B2 |
| Quelldatensatz | uspto-grants-2007_07 |
| ORD ID | ord-5c883ce5096b421db270727eb8e222ea |
| Quellennotiz | uspto-grants-2007_07 |