Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Iodide | HCID 4875 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | p-Fluorophenyl 4-piperidyl ketone hydrochloride | HCID 3084438 | — |
| Edukt | 1-(4-chlorobutyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 13360889 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Methyl Isobutyl Ketone | HCID 7909 | — |
| Produkt | HCID 54155158 | HCID 54155158 | 30% |
Reaktionsschritte
A mixture of 4 parts of 1-(4-chlorobutyl)-1,3-dihydro-2H-benzimidazol-2-one, 4 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 10 parts of sodium carbonate, 0.2 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The solid residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 2 parts (30%) of 1-{4-[4-(4-fluorobenzoyl)-1-piperidinyl]butyl} -1,3-dihydro-2H-benzimidazol-2-one; mp. 176.5° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04035369 |
|---|
| Quelldatensatz | uspto-grants-1977_07 |
|---|
| ORD ID | ord-fc9d249e84de44eebf843f8c59c1d2ba |
|---|
| Quellennotiz | uspto-grants-1977_07 |
|---|