HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 2-(2-Chloro-4-cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Sulfuryl chloride | HCID 24648 | — |
| Edukt | 2-(4-Cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one | HCID 58287277 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 2-(2-Chloro-4-cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one | HCID 58287272 | 30,8% |
Reaktionsschritte
A mixture of 0.275 g (1 mmol) 2-(4-Cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one. 1.57 g (11.3 mmol) sulfuryl chloride and 0.154 g (1.52 mmol) NEt3 in 50 mL CHCl3 was stirred at room temperature. After evaporation of the volatiles the residue was taken up in DMF and subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and NEt3. The product containing fractions were evaporated to yield 94 mg (30%) of the title compound as light yellow gum. MS m/e: 305.1 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08389539B2 |
| Quelldatensatz | uspto-grants-2013_03 |
| ORD ID | ord-87155c578a514598b98c3ac5dc7a05fa |
| Quellennotiz | uspto-grants-2013_03 |