HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-(1,2-Benzoxazol-3-yl)acetic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Hydroxylamine, sulfate (1:1) | HCID 159255 | — |
| Edukt | 4-Hydroxycoumarin | HCID 54682930 | — |
| Katalysator | Edta disodium | HCID 44120005 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | 2-(1,2-Benzoxazol-3-yl)acetic acid | HCID 301729 | — |
Reaktionsschritte
A mixture of hydroxylamine sulfate (344.0 g), water (904 ml) and a 25% aqueous sodium hydroxide solution (456 ml) is stirred, and thereto are added 4-hydroxycoumarin (168.0 g) and ethylenediaminetetraacetic acid disodium salt dihydrate (3.2 g), and the mixture is stirred with heating at 84° C.-86° C. for 4 hours. The reaction mixture is cooled, and thereto is added 1,2-dichloroethane (240 ml). The mixture is stirred, and the aqueous layer is collected. The pH value of the aqueous layer is adjusted to pH 1-2 with 25% sulfuric acid, and the precipitated crystals are collected by filtration, washed with water, and dried with air at 60° C. for 15 hours to give 1,2-benzisoxazole-3-acetic acid (170.4 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07262304B2 |
| Quelldatensatz | uspto-grants-2007_08 |
| ORD ID | ord-aad2945f10194c0d86862b7871db640d |
| Quellennotiz | uspto-grants-2007_08 |