HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
p-Xylyl bromide → 5-n-Butyl-2,4-dihydro-2-(4-methylbenzyl)-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | p-Xylyl bromide | HCID 7721 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4'-[(3-butyl-5-oxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)methyl]biphenyl-2-carbonitrile | HCID 14951052 | — |
| Produkt | 5-n-Butyl-2,4-dihydro-2-(4-methylbenzyl)-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one | HCID 19939395 | 76% |
Reaktionsschritte
The alkylation of 5-n-butyl-4-[(2'-cyanobiphenyl-4-yl)methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one with 4-methylbenzyl bromide was carried out as described in Example 3, Step A, except that no excess sodium hydride was used. After work-up, flash chromatography of the crude product on silica gel (eluting with 0.6% methanol in CH2Cl2) provided a 76% yield of the title compound as a clear oil, homogeneous by TLC (98:2 CH2Cl2 --MeOH), mass spectrum (FAB) m/e 437 (M+1)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05411980 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-7add0288a72b49038c85dfb38b0c0104 |
| Quellennotiz | uspto-grants-1995_05 |