HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → 2,6-Di-sec-butylphenol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Carbamic acid 2,6-di-sec-butylphenyl ester | HCID 66725334 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 2,6-Di-sec-butylphenol | HCID 21685 | 100,3% |
Reaktionsschritte
R-(+)-1-Phenyl-ethyl)-carbamic acid (−) 2,6-di-sec-butylphenyl ester (1b) (4.1 g, 11.6 mmol) was dissolved in a 100 ml 1:1 mixture of dioxane: 1M NaOH aq. The reaction mixture was stirred at 70° C. for 15 min. Volatiles were removed at reduced pressure to a volume of ˜50-70 ml. The pH was adjusted to 3-4 with 1M HCl. The phenol was extracted with ether (3×50 ml), washed with 1 M HCl, brine and dried over anhydrous MgSO4. Evaporation yielded crude yellow oil (2.4 g, ˜100%). Vacuum distillation was performed (120-125° C./˜5 mm) (2.1 g, 89%). Optical rotation: α20D=−14.11° (c=2, pentane).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08871815B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-adf940e11111468e8d881097bac8f4c3 |
| Quellennotiz | uspto-grants-2014_10 |