Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | Chloroacetyl chloride | HCID 6577 | — |
| Edukt | Pyrimidin-5-amine | HCID 344373 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | 2-Chloro-N-pyrimidin-5-yl-acetamide | HCID 20208139 | — |
Reaktionsschritte
5-Aminopyrimidine (450 mg) was suspended in DCE (2 mL) and acetonitrile (2 mL) in a microwave vial. Chloroacetyl chloride (0.377 mL) was added with stirring. The vial was sealed and the reaction mixture was heated in the microwave at 80° C. for 5 minutes. The solid was filtered off, washed with acetonitrile (2×5 mL), DCE (2×5 mL) and pentane (2 ×30 mL) and then partioned between saturated sodium bicarbonate and DCE (50 mL/50 mL) ensuring the aqueous layer was still basic. The organic layer was separated and the aqueous layer was extracted with DCE (2×75 mL). The combined organic layer was dried over magnesium sulfate and evaporated to give the sub-titled compound (200 mg) as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08329729B2 |
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| Quelldatensatz | uspto-grants-2012_12 |
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| ORD ID | ord-4a31dca5b97042f5afd384119e29a258 |
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| Quellennotiz | uspto-grants-2012_12 |
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