Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 5-Fluoro-2-methylbenzothiazole | HCID 597437 | — |
| Lösungsmittel | Ethylene Glycol | HCID 174 | — |
| Lösungsmittel | Sodium Hydroxide | HCID 14798 | — |
| Produkt | 2-Amino-4-fluorobenzene-1-thiol | HCID 11105480 | — |
Reaktionsschritte
A solution of 5-fluoro-2-methylbenzo[d]thiazole (1.2 g, 7.18 mmol) in ethylene glycol and NaOH (5N, 2 ml) was degassed under N2 for 10 min, then refluxed at 129° C. for 3 hours. The solution was cooled to 0° C. and then acidified to pH 3˜4 using c. HCl. The mixture was extracted with EtOAc (2×50 ml). The organic layer was washed with brine and dried with Na2SO4 and concentrated in vacuo. The crude residue (1.01 g, 98%) was used directly in the next step without purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08822530B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-38e9a4925477471da7fb67a13f1514d8 |
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| Quellennotiz | uspto-grants-2014_09 |
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