Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethylamine | HCID 6341 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Acetylacetone | HCID 31261 | — |
| Edukt | 5-Methyl hydrogen L-glutamate | HCID 68662 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | L-Theanine | HCID 439378 | 91% |
Reaktionsschritte
First, 320 g (1.983 mol) of L-glutamic acid-γ-methyl ester was suspended in 500 g of methanol. To this, 219 g (2.186 mol, 1.1 eq.) of acetylacetone and 200 g (1.983 mol, 1 eq.) of triethylamine were added. The mixture was stirred at 60° C. for one hour. Subsequently, 1,277 g (19.8 mol) of 70% ethylamine was added to the mixture. After the mixture was allowed to react for 6 hours, the reaction solution was heated under normal pressure. In this manner, 667 g of excessive ethylamine was recovered and deprotection was performed at the same time. To the slurry of the theanine precipitated, 1 L of 2-propanol was added. The crystal was filtrated by suction and washed with 200 mL of 99.5% ethanol to obtain theanine (314.3 g) as a white crystal substance (yield: 91%). The obtained theanine had the same purity as high as in Example 1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08178722B2 |
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| Quelldatensatz | uspto-grants-2012_05 |
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| ORD ID | ord-d01eb78e7f554425aa2459a45789765c |
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| Quellennotiz | uspto-grants-2012_05 |
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