HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 1-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | 2-Ethenyl-6-methylpyridine | HCID 70735 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | 4-(4-Methylsulfonylaminophenylsulfonyl)piperidine hydrochloride | HCID 18539239 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine | HCID 15027722 | 64% |
Reaktionsschritte
0.60 g (1.86 mmol) of 4-(4-methylsulfonylaminophenylsulfonyl)piperidine hydrochloride obtained in Example 5, 0.44 g (3.72 mmol) of 6-methyl-2-vinylpyridine and 0.31 g of sodium acetate were suspended in 10 ml of a mixture of methanol with water (1:1) and the suspension was refluxed for 2 h. The reaction liquid was filtered and the filtrate was concentrated to give a residue. After extraction with dichloromethane followed by washing with water, the organic layer was concentrated to precipitate white crystals. The crystals were collected by filtration and recrystallized from ethyl acetate to give 0.52 g (yield: 64%) of the intended compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05162347 |
| Quelldatensatz | uspto-grants-1992_11 |
| ORD ID | ord-e55315fc54894454a029f58dd9684473 |
| Quellennotiz | uspto-grants-1992_11 |