HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cyanogen Bromide → 1'-Cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine]
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cyanogen Bromide | HCID 10476 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1'-Methyl-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine] | HCID 12801596 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 1'-Cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine] | HCID 12801615 | — |
Reaktionsschritte
A solution of 18.23 g of 1-(2-nitrophenyl)-1'-methylspiro[indoline-3,4'-piperidine] of Example 15 in 100 ml of chloroform is added dropwise over 50 minutes to a rapidly stirred slurry of 11.65 g of potassium carbonate and 8.94 g of cyanogen bromide in 100 ml of chloroform under nitrogen. After heating at reflux for 2.75 hours, the cooled product is washed with 10% sodium hydroxide and water, dried over anhydrous magnesium sulfate and concentrated to yield a crude solid which is chromatographed on silica gel (650 g) using ether-chloroform and is then recrystallized from ether-dichloromethane to yield a solid, mp 148°-150° C. of 1'-cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04408050 |
| Quelldatensatz | uspto-grants-1983_10 |
| ORD ID | ord-ad5362cfe95144379cb318f46f10beee |
| Quellennotiz | uspto-grants-1983_10 |