Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 4-chloro-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine | HCID 239498 | — |
| Edukt | HCID 178479279 | HCID 178479279 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | HCID 178505624 | HCID 178505624 | 100,6% |
Reaktionsschritte
A mixture of 0.52 g trans-4-[2-fluoro-2-(2-fluorophenyl)ethoxy]-cyclohexanamine hydrochloride, 0.46 g of 4-chloro-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine, and 1 g of powdered sodium carbonate in 25 mL of 2-propanol was heated to 80° C. under nitrogen overnight. The mixture was cooled, filtered and the solid washed with 3×50 mL portions of 10% methanol in chloroform. The combined extracts were concentrated under reduced pressure. Chromatography over silica gel eluting with a gradient of 50%-100% ethyl acetate in hexane gave 0.82 g of product as a white solid: MS (m+1)=458.4.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07452893B2 |
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| Quelldatensatz | uspto-grants-2008_11 |
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| ORD ID | ord-f118c036d90f425b928d66ab02323387 |
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| Quellennotiz | uspto-grants-2008_11 |
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