HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2,2-Dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Pivaloyl chloride | HCID 62493 | — |
| Edukt | 8-Ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one | HCID 59614581 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2,2-Dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester | HCID 58031265 | — |
Reaktionsschritte
To 143 mg of 8-ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one in 1 ml of tetrahydrofuran were added 36 μl of pyridine and 53 μl of pivaloyl chloride. After stirring at room temperature for 20 hours, water and ethyl acetate were added and the phases separated. The aqueous phase was extracted with ethyl acetate, the combined organic phases dried with sodium sulfate, filtered and concentrated. Chromatography (heptane/ethyl acetate 2:1) yielded 117 mg of 2,2-dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester (title compound A54) as a solid, mp: 230-231° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08415369B2 |
| Quelldatensatz | uspto-grants-2013_04 |
| ORD ID | ord-e070a7aaa4b7451a82b4176890038241 |
| Quellennotiz | uspto-grants-2013_04 |