関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 5-Amino-2,2-difluoro-1,3-benzodioxole | HCID 2736893 | — |
| 反応物 | N-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-yl)-1-chloro-6-methylisoquinolin-5-amine | HCID 59627378 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | HCID 68779395 | HCID 68779395 | — |
反応手順
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+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08557830B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-f9900f46dbbd4efc822e74401859a9bf |
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| 出典メモ | uspto-grants-2013_10 |
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