Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Nitric Acid | HCID 944 | — |
| Edukt | 2,3-Dichlorobenzaldehyde | HCID 35745 | — |
| Edukt | 2,3-Dichloro-5-nitrobenzaldehyde | HCID 18767162 | — |
| Edukt | 4-Prenylphlorisovalerophenone | HCID 25200610 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 2,3-Dichloro-6-nitrobenzaldehyde | HCID 11218271 | — |
Reaktionsschritte
A solution of 40 g of 2,3-dichlorobenzaldehyde (compound IX) in 160 mL of concentrated sulfuric acid (95-98% w/w) is heated to 40° C. and stirred to form a solution, then cooled to 20-25° C. Concentrated nitric acid (69-71% w/w; 24.7 g) is added to this solution over 20 minutes (an ice bath is used to maintain a reaction temperature of 20-30° C.). The reaction mixture is stirred at room temperature for 1 hour, and then added in portions to 600 mL of water. The resulting suspension is stirred for 2 hours and filtered. The filter cake is washed (3×50 mL of water). The filter cake is agitated with 200 mL of water for 2 hours and filtered. The filter cake is washed (3×50 mL of water) and dried in vacuo to give a mixture of the compound X and the isomer, 2,3-dichloro-5-nitrobenzaldehyde.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06653500B2 |
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| Quelldatensatz | uspto-grants-2003_11 |
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| ORD ID | ord-229204585ba346d59904f042af95521b |
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| Quellennotiz | uspto-grants-2003_11 |
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