HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → O-3-methoxy-5-methylphenyl dimethylcarbamothioate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Dabco | HCID 9237 | — |
| Edukt | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| Edukt | 3-Methoxy-5-Methylphenol | HCID 76674 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | O-3-methoxy-5-methylphenyl dimethylcarbamothioate | HCID 58294848 | 91,5% |
Reaktionsschritte
To a mixture of 3-methoxy-5-methylphenol (7) (3.39 g, 24.5 mmol) and 1,4-diazabicyclo[2.2.2]octane (5.50 g, 49.0 mmol) in DMF (20 mL) was added dimethylthiocarbamoyl chloride (8) (6.06 g, 49.0 mmol) portionwise. The reaction mixture was stirred at room temperature overnight and 500 mL of ether was added. The organics were washed with water (150 mL), brine (2×50 mL), dried (Na2SO4), and concentrated. Purification by chromatography on silica gel (Hexanes/EtOAc, 4:1) gave O-3-methoxy-5-methylphenyl dimethylcarbamothioate (9) (5.05 g, 91%) as a colourless solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08101605B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-3123dddee2e9461a81930c4e3de5ee81 |
| Quellennotiz | uspto-grants-2012_01 |