Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Nitric Acid | HCID 944 | — |
| Edukt | 2,3,6-Trichlorobenzoic acid | HCID 5759 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 3-Nitro-2,5,6-trichlorobenzoic acid | HCID 19094239 | 94% |
Reaktionsschritte
2,3,6-Trichlorobenzoic acid (20.84 g, 92.4 mmol, prepared by the method of M. T. Goebel, U.S. Pat. No. 3,391,185, E.I. DuPont, Jul. 2, 1968) was stirred at 40°-45° C. in 89.1 mL of concentrated sulfuric acid. A solution containing 23.2 g of concentrated sulfuric acid and 23.2 g of fuming nitric acid was added at a rate so to maintain the temperature between 40°-45° C. An additional 20 mL of concentrated sulfuric acid was added. The reaction mixture was stirred at 43° C. for 1.5 hours and then poured over ice water. The resulting crystals were filtered and recrystallized from toluene-hexane to give 23.40 g (94%) of product; mp 149°-151° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05294631 |
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| Quelldatensatz | uspto-grants-1994_03 |
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| ORD ID | ord-2af3472b9a024c70bc69434d4d87d6a0 |
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| Quellennotiz | uspto-grants-1994_03 |
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