HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → cis-1-(4-Chlorophenylsulfonyl)-2,6-dimethylpiperidin-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 4-Chlorobenzenesulfonyl chloride | HCID 7398 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | cis-2,6-Dimethylpiperidin-4-one | HCID 13561054 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | cis-1-(4-Chlorophenylsulfonyl)-2,6-dimethylpiperidin-4-one | HCID 59342367 | — |
Reaktionsschritte
The crude cis-2,6-dimethylpiperidin-4-one 91 from previous experiment (1.1 g, 8.6 mmol) was dissolved in CH2Cl2 (50 mL) and triethylamine (5 mL, 35 mmol) was added. Stirred solution was treated with 4-chlorobenzenesulfonyl chloride (2.2 g, 9.5 mmol). The mixture was stirred for 24 hr then was divided between water (100 mL) and CH2Cl2 (100 mL). Organic layer was washed with 0.2 N citric acid, water, brine and dried over anhydrous Na2SO4. The solution was filtered and evaporated. The residue was purified by flash chromatography, eluting with EtOAc-hexane (1:3) mixture. Yield 60 mg (2% after two steps).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732609B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-71b99c62f1f846faa023e22183d00378 |
| Quellennotiz | uspto-grants-2010_06 |