Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Chloroacetyl chloride | HCID 6577 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | N-(2-Hydroxyethyl)aniline | HCID 31235 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 4-Phenylmorpholin-3-ON | HCID 5153080 | — |
Reaktionsschritte
In a 26-liter tank, 1.65 kg (12.0 mol) of 2-anilinoethanol are dissolved at room temperature in 1.53 l of ethanol and subsequently admixed with 4.58 l of water with stirring. The solution is heated to 38° C. 4.07 kg (3.0 equivalents) of chloroacetyl chloride and 6.60 kg of 45% sodium hydroxide solution (6.2 equivalents) are then added simultaneously at an internal temperature of 38 to 43° C. within 60 to 80 minutes, so that the pH is kept between 12 and 12.5. The mixture is stirred at a pH of 12 to 12.5 for 10 minutes, then cooled to 2° C. and stirred at this temperature for 30 minutes. The precipitated product is filtered off and washed twice with 3.3 kg each time of demineralized water at 2° C. The moist product is dried to constant mass at 50° C. under reduced pressure.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07598378B2 |
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| Quelldatensatz | uspto-grants-2009_10 |
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| ORD ID | ord-a9b7726ff18a492db93b7bb2fd6fe49b |
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| Quellennotiz | uspto-grants-2009_10 |
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