HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → Methyl 3-amino-2-methyl-6-thiocyanatobenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Bromine | HCID 24408 | — |
| Edukt | Sodium Bromide | HCID 253881 | — |
| Edukt | Sodium thiocyanate | HCID 516871 | — |
| Edukt | 3-Amino-2-methylbenzoic acid methyl ester | HCID 3801025 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | Methyl 3-amino-2-methyl-6-thiocyanatobenzoate | HCID 14801188 | 91,2% |
Reaktionsschritte
While maintaining a solution comprising 27.7 g of methyl 3-amino-2-methylbenzoate, 41.5 g of sodium thiocyanate and 250 ml of methanol at a temperature of not higher than 0° C., 100 ml of sodium bromide-saturated methanol with 28.1 g of bromine was slowly dropwise added thereto. The mixture was stirred at room temperature for 3 hours and then poured into 1 liter of ice water. The solution was neutralized with sodium carbonate and then extracted with chloroform. The extract was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. Then, the solvent was distilled off to obtain 34.0 g of the desired product as an oily substance.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04885022 |
| Quelldatensatz | uspto-grants-1989_12 |
| ORD ID | ord-787fce87cce8402592768e9530675cb5 |
| Quellennotiz | uspto-grants-1989_12 |