HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → HCID 178490206, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Thioglycolic Acid | HCID 1133 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 4-(Chloromethyl)-2-nitroanisole | HCID 80785 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178490206 | HCID 178490206 | 95% |
Reaktionsschritte
To a cold solution of sodium hydroxide (9.75 g, 240 mmol) in methanol (200 mL), thioglycollic acid (11.25 g, 120 mmol) was added slowly over 30 minutes. Sodium thioglycollate precipitated was dissolved by stirring and warming up the solution. The solution was cooled to room temperature and 4-methoxy-3-nitrobenzyl chloride (30.0 g, 120 mmol) was added in portions to reduce the intensity of exothermic reaction. The reaction mixture was then refluxed for 4 hours, cooled and poured onto crushed ice (1 Kg) containing hydrochloric acid (50 mL). The precipitate formed was filtered, washed with ice cold water and dried under vacuum. (30.0 g, 95% yield) m.p. 130-132° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08273787B2 |
| Quelldatensatz | uspto-grants-2012_09 |
| ORD ID | ord-db2d356282fa4cd3944d1d7e6e4b221b |
| Quellennotiz | uspto-grants-2012_09 |