HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 3-((4-Bromo-3,5-dimethylphenoxy)methyl)-3-methyloxetane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| Edukt | Oxetane, 3-(bromomethyl)-3-methyl- | HCID 144860 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-((4-Bromo-3,5-dimethylphenoxy)methyl)-3-methyloxetane | HCID 86697102 | — |
Reaktionsschritte
To a solution of 4-bromo-3,5-dimethylphenol (3.0 g) and K2CO3 (5.5 g) in N,N-dimethylformamide (10 mL) is added 3-(bromomethyl)-3-methyloxetane (2.95 g). The mixture is stirred for 12 hours at room temperature and then partitioned between saturated aqueous NaHCO3 solution and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are dried (MgSO4). The solvent is evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 100:0→70:30) to give the title compound. Yield: 3.5 g; LC (method 4): tR=1.81 min; Mass spectrum (ESI+): m/z=285 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08642585B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-7d867147ffd541b38140cb598cd36b86 |
| Quellennotiz | uspto-grants-2014_02 |