Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Dimethyl Sulfone | HCID 6213 | — |
| Edukt | Ethyl 2-amino-4-methylthiophene-3-carboxylate | HCID 521132 | — |
| Edukt | Chloroformamidinium chloride | HCID 3084509 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178431879 | HCID 178431879 | 87,9% |
Reaktionsschritte
A mixture of ethyl 2-amino-4-methylthiophene-3-carboxylate (2.0 g, 11.7 mmol), chloroformamidine hydrochloride (3.357 g, 29.0 mmol) and dimethylsulfone (5.489 g, 58.4 mmol) was heated at 135° C. for 45 minutes. Water was added and the mixture was cooled down to room temperature. An aqueous ammonia solution was added to adjust the solution to pH 9. The precipitate was filtered off, yielding the title compound (1.863 g) as a white powder. 13C NMR δ (75 MHz, DMSO-d6) 168.98, 159.12, 153.21, 133.26, 114.37, 110.81, 16.35. MS (m/z) 182 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09227984B2 |
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| Quelldatensatz | uspto-grants-2016_01 |
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| ORD ID | ord-c1695a9815aa42c2b10daecd926f3082 |
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| Quellennotiz | uspto-grants-2016_01 |
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