Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Nitric Acid | HCID 944 | — |
| Edukt | 2-Bromo-6-nitrotoluene | HCID 123537 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 1-Bromo-2-methyl-3,4-dinitrobenzene | HCID 15889633 | 77% |
Reaktionsschritte
To a cold (0° C.) solution of 2-bromo-6-nitrotoluene (43.2 g, 0.2 mol) in con H2SO4 (600 mL) was added HNO3 (37 g, 0.24 mol) in small portions with efficient agitation while maintaining the temperature at 0-10° C. The reaction mixture was allowed to slowly warm to RT with stirring overnight then poured into crushed ice (1600 g). The solid was collected by filtration, thoroughly washed with water and dried in air. The crude material was recrystallised from EtOAc/hexanes to afford 40 g (77%) of 1-bromo-2-methyl-3,4-dinitrobenzene (154) as a pale white solid: MS (ESI) m/z=262 [M+1]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08637537B2 |
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| Quelldatensatz | uspto-grants-2014_01 |
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| ORD ID | ord-470db701f47c412ab0bb045e48df4d5f |
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| Quellennotiz | uspto-grants-2014_01 |
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