HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → HCID 19770510, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Thioglycerol | HCID 7291 | — |
| Edukt | 2-Hydroxy-5-nitrobenzyl bromide | HCID 13044 | — |
| Edukt | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 19770510 | HCID 19770510 | — |
Reaktionsschritte
13.2 g of potassium hydroxide pellets (85 %) are heated to 45° C. in 27 g of thioglycerol. 10 ml of N-methylpyrrolidone are added followed portionwise over 30 minutes by 0.1 mole (23.2 g) of 2-hydroxy-5-nitrobenzyl bromide. The temperature of 67°-70° C. which is obtained is maintained for 30 minutes after the end of addition. The reaction mixture is diluted with 300 g of iced water. After neutralizing with acetic acid, the expected product precipitates. After filtering off, followed by drying at 45° C. under vacuum the product obtained is recrystallized from isopropyl acetate. It melts at 130° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05202487 |
| Quelldatensatz | uspto-grants-1993_04 |
| ORD ID | ord-a0c10528a11c484997247d82bc683b3f |
| Quellennotiz | uspto-grants-1993_04 |