Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Sulfite | HCID 24437 | — |
| Edukt | Iodine chloride | HCID 24640 | — |
| Edukt | 6-Chloro-2-methylpyrimidin-4-amine | HCID 286754 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 88580856 | HCID 88580856 | 80% |
Reaktionsschritte
Combine 6-chloro-2-methylpyrimidin-4-amine (708 g, 4.93 mol) and MeOH (7.08 L) in a 20 L round bottom flask equipped with a mechanical stirrer. Cool to 0-5° C. Add iodine monochloride (4.806 kg, 29.6 mol) dissolved in MeOH (6 L) using an addition funnel over a period of 1 h. Warm the reaction mixture to RT and stir at RT for 16 h. Cool the reaction mixture to 0-5° C. and add sodium sulfite (46 L, 20% aqueous solution). Filter the resulting solid and wash with water (2 L) followed by hexane (3 L). Dry the solid under vacuum to afford the title compound as a white solid (1061 g, 80%). LC-ES/MS m/z 269.9 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09035051B1 |
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| Quelldatensatz | uspto-grants-2015_05 |
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| ORD ID | ord-f70f3c19650644a99b8c0b25040f25f2 |
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| Quellennotiz | uspto-grants-2015_05 |
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