Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-Methoxyimino-5-methylthiochroman-6-carboxylic acid-1,1-dioxide | HCID 53971540 | — |
| Edukt | HCID 178418331 | HCID 178418331 | — |
| Lösungsmittel | 2-Methyl-2-butanol | HCID 6405 | — |
| Produkt | HCID 178418231 | HCID 178418231 | 72,9% |
Reaktionsschritte
0.9 Gram (3.2 mmol) of the 4-methoxyimino-5-methylthiochroman-6-carboxylic acid-1,1-dioxide and 0.44 g (3.9 mmol) of 1-ethyl-5-hydroxypyrazol were dissolved in 5 ml of t-amyl alcohol, and 0.81 g (3.9 mmol) of DCC(dicyclohexyl-carbodiimide) was added at room temperature. The mixture was stirred at room temperature for 2 hours, then, 0.74 g (5.4 mmol) of potassium carbonate was added, and the mixture was allowed to react at 90° C. for 8 hours. After the reaction, the solvent was distilled off, ethyl acetate was added, and the mixture was extracted with a 5% potassium carbonate aqueous solution. An aqueous layer was neutralized with concentrated hydrochloric acid, and extracted with ethyl acetate. The extract was washed with a saturated sodium hydroxide aqueous solution, dried over sodium sulfate and concentrated to give 0.88 g (yield 72%) of 4-methoxyimino-5-methyl-6 -(1-ethyl-5-hydroxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05849926 |
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| Quelldatensatz | uspto-grants-1998_12 |
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| ORD ID | ord-de65b6be9942400f8d6080f2f3e6e3b6 |
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| Quellennotiz | uspto-grants-1998_12 |
|---|