HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetonitrile → 5-bromo-N-(5-(4-methoxyphenyl)-1H-pyrazol-3-yl)pentanamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 5-Bromovaleryl chloride | HCID 521173 | — |
| Edukt | 3-Amino-5-(4-methoxyphenyl)pyrazole | HCID 2756469 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-bromo-N-(5-(4-methoxyphenyl)-1H-pyrazol-3-yl)pentanamide | HCID 57780044 | 70% |
Reaktionsschritte
A solution of 5-(4-methoxyphenyl)-1H-pyrazol-3-amine and diisopropylethylamine in 10 volumes of a 9:1 mixture of acetonitrile:DMF was cooled to −10° C. 5-Bromovaleryl chloride was added dropwise over a minimum of 3 hr at −10° C. The resulting solution was held at −10° C. until reaction completion, generally 2 hr. The reaction mixture was quenched with water. The product was isolated by filtration, washed with water, TBME and suction dried. The product-wet cake was purified by re-slurrying in TBME at 35° C. for a minimum of 2 hr. The yield was 70-80%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08163729B2 |
| Quelldatensatz | uspto-grants-2012_04 |
| ORD ID | ord-683875a419054f5bad35ae15022f4db4 |
| Quellennotiz | uspto-grants-2012_04 |