Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chloroacetic Acid | HCID 300 | — |
| Edukt | Diethylamine | HCID 8021 | — |
| Lösungsmittel | tert-Butyl methyl ether | HCID 15413 | — |
| Produkt | N,N-Diethylglycine | HCID 74151 | — |
Reaktionsschritte
Diethylamine (9.5 L) was charged into a 20 L glass-lined reactor and cooled to 3° C. Chloroacetic acid (1.21 kg) in MTBE (1.8 L) was added over 1 hour with cooling—the temperature rose to 16° C. during the addition. The mixture was warmed to 20° C., stirred over night and concentrated on rotary evaporator giving yellow oil. This oil was re-concentrated with iPrOAc, mixed with iPrOAc (4.5 L) and stirred over night. The off-white hygroscopic precipitate was filtered, washed with iPrOAc (1.5 L) and immediately placed into a drying cabinet to avoid deliquescence. After drying, titled product was obtained (820 g, Y=49%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08227428B2 |
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| Quelldatensatz | uspto-grants-2012_07 |
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| ORD ID | ord-27b689454e0a40369c14617ecde24831 |
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| Quellennotiz | uspto-grants-2012_07 |
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