関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,3-Diiodopropane | HCID 12314 | — |
| 反応物 | 3-(Benzyloxy)pyridin-2-ol | HCID 15666452 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(benzyloxy)-1-(3-iodopropyl)pyridin-2(1H)-one | HCID 59537189 | 10% |
反応手順
To a solution of 1,3-diiodopropane (7.1 mL, 63 mmol) in tetrahydrofuran (50 mL) was added 3-(benzyloxy)pyridin-2(1H)-one (1.28 g, 6.3 mmol) and Na2CO3 (0.67 g, 6.3 mmol). The mixture was then stirred at 70° C. for 1 day. Reaction progress was monitored by ES-MS. After ESMS showed essentially complete consumption of the starting material 3-(benzyloxy)pyridin-2(1H)-one, the reaction was stopped. Then the reaction mixture was filtered, concentrated, and subjected to flash column chromatography (eluent: hexane:ethylacetate 1:1). Compound 7 was obtained (240 mg, 10% yield). Analysis: ES-MS (positive ion in MeOH/H2O): m/z=370.2, ([M+H]+, calculated: 370.03).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08598381B2 |
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| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-8ed2954d6a1a413c8a84075910a87a2c |
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| 出典メモ | uspto-grants-2013_12 |
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