HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Chloride → HCID 57457055, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | Sodium Azide | HCID 33557 | — |
| Edukt | 4-[(Cyanomethyl)sulfanyl]benzoic acid | HCID 20114986 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 57457055 | HCID 57457055 | 16% |
Reaktionsschritte
A mixture of 4-cyanomethylsulfanylbenzoic acid (27.2 g, 0.14 mol), sodium azide (11.8 g, 0.18 mol) and ammonium chloride (9.7 g, 0.18 mol) in DMF (1000 mL) was refluxed overnight under N2. The mixture was concentrated in vacuo. The residue was suspended in cold water and extracted with diethyl ether. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated in vacuo. Water was added and the precipitate was filtered off. The aqueous layer was concentrated in vacuo, water was added and the precipitate filtered off. The combined impure products were purified by column chromatography using DCM:MeOH=9:1 as eluent, affording the title compound (5.2 g, 16%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07879893B2 |
| Quelldatensatz | uspto-grants-2011_02 |
| ORD ID | ord-e04c3cbe05ce4ac98a80b4b8b61b3ed7 |
| Quellennotiz | uspto-grants-2011_02 |