HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 4-Hydroxy-4-(dimethylamino-ethyl)-3,5-dimethyl-2,5-heptadiene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 2-Bromobut-2-ene | HCID 20910 | — |
| Edukt | beta-Alanine, N,N-dimethyl-, ethyl ester | HCID 88372 | — |
| Edukt | Lithium | HCID 3028194 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 4-Hydroxy-4-(dimethylamino-ethyl)-3,5-dimethyl-2,5-heptadiene | HCID 54506043 | — |
Reaktionsschritte
2-bromo-2-butene (108 g; 0.800 mol) was added to 10.0 g of lithium (1.43 mol) in diethyl ether (300 ml) in about 30 minutes with reflux. After stirring overnight (17 hours), ethyl-3-(N,N-dimethylamino)propionate (52.0 g; 0.359 mol) was added to the reaction mixture in about 15 minutes. After stirring for 30 minutes at room temperature 200 ml of water was added dropwise. After separation the water phase was extracted two times with 50 ml of CH2Cl2. The organic phase was reduced by evaporation and the residue was distilled at reduced pressure. The yield was 51.0 g (67%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05986029 |
| Quelldatensatz | uspto-grants-1999_11 |
| ORD ID | ord-d5a0a84cc3ec4bed810ffba6e19bbaf3 |
| Quellennotiz | uspto-grants-1999_11 |