Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 3,5-Dichloroanthranilic acid | HCID 76036 | — |
| Produkt | Methyl 2-amino-3,5-dichlorobenzoate | HCID 613050 | 78,6% |
Reaktionsschritte
To a 500 mL round-bottom flask, 0.2 mol of 2-amino-3,5-dichlorobenzoic acid having a structural formula of IV-4, 300 mL of methanol, and 5 mL of concentrated sulfuric acid were added, heated to 64° C. and reacted for 12 hours (into which 3 mL of concentrated sulfuric acid was added twice), after cooling most of the solvent was removed under reduced pressure, and 300 mL of water was added, the pH was adjusted to 9-10 with a saturated sodium hydroxide solution, extracted with 200 mL of ethyl acetate, washed with water for one time, dried over anhydrous sodium sulfate, filtered and the solvent was remove to obtain a crude product, 34.6 grams of 2-amino-3,5-dichlorobenzoic acid methyl ester having a structure as shown by VIII-1 was obtained by column chromatography, and the yield was 78.6%;
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09301529B2 |
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| Quelldatensatz | uspto-grants-2016_04 |
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| ORD ID | ord-215dc61984c343fa8353c7f55196dbf9 |
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| Quellennotiz | uspto-grants-2016_04 |
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