Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Chloroacetone | HCID 6571 | — |
| Edukt | 2-Nitrophenol | HCID 6947 | — |
| Edukt | Sodium Bromide | HCID 253881 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Katalysator | Tributylmethylammonium chloride | HCID 91822 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 2-Propanone, 1-(2-nitrophenoxy)- | HCID 79239 | — |
Reaktionsschritte
The o-nitrophenoxyacetone is prepared by heating with agitation for five hours at about 65° C. a mixture which consists of 421.6 g (3.006 moles) of o-nitrophenol, 297.8 g (3.09 moles) of chloroacetone, 37.2 g (96%, 0.3615 moles) of sodium bromide, 277.2 g (3.3 moles) of sodium bicarbonate, 21.8 g (0.0647 moles) of aqueous tributylmethylammonium chloride (TBMAC), and 829 g of toluene. There is then added 9.0 g (0.093 mole) of additional chloroacetone to the mixture which is further heated at 65° C. for 2.5 hours (note, sample analysis indicated that the reaction was complete after 1.5 hours). There is then added, 570 g of water and the pH of the mixture is adjusted to 6.5–7 at 55° C. to 60° C. upon addition of 55 g of a 10% HCl solution. The phases are allowed to separate and the aqueous phase is removed.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06977299B2 |
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| Quelldatensatz | uspto-grants-2005_12 |
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| ORD ID | ord-98cbcdae6c2545c8bc14097ac9f282d3 |
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| Quellennotiz | uspto-grants-2005_12 |
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