HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Hydroxide → 2-(5-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| Edukt | 2-Amino-5-isopropylbenzonitrile | HCID 21093463 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | 2-(5-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile | HCID 58625957 | 16,4% |
Reaktionsschritte
Heat a solution of 2-amino-5-isopropyl-benzonitrile (1.21 g, 7.55 mmol) with 2,4-difluoro-1-nitro-benzene (1.20 g, 7.55 mmol) and lithium hydroxide (0.54 g, 22.66 mmol) in DMSO (15 ml) to 70° C. for 18 hours. Cool the reaction to ambient temperature and then pour into approximately 200 ml of ice water and stir for one hour. The title compound precipitates and is colleted by filtration. Purify the solid via flash chromatography eluting with a 95% hexanes: 5% ethyl acetate mobile phase to obtain 0.372 g (1.24 mmol, 16% yield) of the title compound as an orange amorphous solid: Mass Spectrum (m/e): 298 (M−1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07384934B2 |
| Quelldatensatz | uspto-grants-2008_06 |
| ORD ID | ord-c4491ebbc188498abc9e2e87309ba20e |
| Quellennotiz | uspto-grants-2008_06 |