Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | 2-Chloroacetophenone | HCID 10757 | — |
| Edukt | (4-Methyl-1,3-thiazol-5-yl)methanol | HCID 10329317 | — |
| Lösungsmittel | tert-Butyl methyl ether | HCID 15413 | — |
| Produkt | HCID 12044346 | HCID 12044346 | — |
Reaktionsschritte
The neat reaction of 4-methyl-5-(hydroxymethyl)thiazole (590 mg, 4.57 mmol) and 2-chloroacetophenone (710 mg, 4.59 mmol) was heated at 110° C. The mixture solidified within 15 minutes. Acetonitrile (10 mL) was added and the mixture refluxed for another 3 hrs. It was cooled to room temperature and tert-butyl methyl ether (5 mL) was added and the reaction mixture was left overnight at room temperature. The product crystallized was filtered and washed well with a mixture of hexanes: EtOAc (1:1, v/v) and dried. It was recrystallized from a mixture of acetonitrile/ethanol/ tert-butyl methyl ether; yield 130 mg (10%); mp.240-242° C. (dec.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07432254B2 |
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| Quelldatensatz | uspto-grants-2008_10 |
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| ORD ID | ord-f934d52eba7a45a0a1443ed52f903fd9 |
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| Quellennotiz | uspto-grants-2008_10 |
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