Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Thiophosgene | HCID 10040 | — |
| Edukt | HCID 178507749 | HCID 178507749 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 178505955 | HCID 178505955 | 78% |
Reaktionsschritte
At 23° C. and under an argon atmosphere, triethylamine (3.34 g; 0.024 mol) is added to a solution containing 2-fluoro-4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (3 g, 0.008 mol) in tetrahydrofuran (120 ml). The reaction medium is cooled down to 0° C. then the thiophosgene compound (1.01 g; 0.0088 mol) is added dropwise. Stirring is maintained at this temperature for thirty minutes then the reaction medium is returned to 23° C. and stirred at this temperature for twenty minutes. 60 ml of water and 150 ml of ethyl ether are added to the reaction medium. The two phases are separated then the organic phase is washed with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate, followed by concentration to dryness then the product obtained is triturated in isopentane with traces of dichloromethane. The solid obtained is filtered then dried. A yellow-coloured powder is obtained with a yield of 78%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08188133B2 |
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| Quelldatensatz | uspto-grants-2012_05 |
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| ORD ID | ord-0ed9b6cc3e93462f884e7425aabdfa9a |
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| Quellennotiz | uspto-grants-2012_05 |
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