Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | 5-Amino-2,2-difluoro-1,3-benzodioxole | HCID 2736893 | — |
| Edukt | N-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-yl)-1-chloro-6-methylisoquinolin-5-amine | HCID 59627378 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Lösungsmittel | Triethylamine | HCID 8471 | — |
| Produkt | HCID 68779395 | HCID 68779395 | — |
Reaktionsschritte
A mixture of 2,2-difluorobenzo[d][1,3]dioxol-5-amine (64 mg, 371 mop, N-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-yl)-1-chloro-6-methylisoquinolin-5-amine (120 mg, 309 μmol) and 2,2,2-trifluoroacetic acid (95 μl, 1238 μmol) in i-PrOH (4 ml) was heated in a microwave reactor at 150° C. for 40 min. The mixture was poured into MeOH (10 ml) and Et3N (0.25 ml) was added. Solvent was removed under vacuum and the product was purified by flash chromatography eluting with MeOH/DCM (1-5%) to give N5-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-yl)-N1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-6-methylisoquinoline-1,5-diamine. MS Found: (ESI pos. ion) m/z 525 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08557830B2 |
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| Quelldatensatz | uspto-grants-2013_10 |
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| ORD ID | ord-f9900f46dbbd4efc822e74401859a9bf |
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| Quellennotiz | uspto-grants-2013_10 |
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