関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-[7-methoxy-4-(tetrahydro-pyran-4-yl)-thiazolo[5,4-c]pyridin-2-yl]-benzamide | HCID 11537949 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 7-Methoxy-4-(tetrahydro-pyran-4-yl)thiazolo[5,4-c]pyridin-2-ylamine | HCID 86038492 | 77.2% |
反応手順
To a stirred suspension of 314 mg (0.85 mmol) N-[7-methoxy-4-(tetrahydro-pyran-4-yl)-thiazolo[5,4-c]pyridin-2-yl]-benzamide in 2.5 ml methanol was added 0.85 ml 5 N aq. sodium hydroxide solution and the resulting solution was then heated at 130° C. for 12 min in a microwave oven. The reaction mixture was then cooled to room temperature and partitioned between tetrahydrofuran and 1 N aq. sodium hydroxide solution. The phases were separated and the organic phase was dried over sodium sulfate and concentrated in vacuo. Flash chromatography (methanol/dichloromethane) afforded 174 mg (77%) 7-methoxy-4-(tetrahydro-pyran-4-yl)-thiazolo[5,4-c]pyridin-2-ylamine as a light yellow crystalline solid. ES-MS m/e (%): 266 (M+H+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07273865B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-2987292ba131407cb468107536d0b4ec |
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| 出典メモ | uspto-grants-2007_09 |
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