関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Methyl 3-chloropropionate | HCID 22321 | — |
| 反応物 | 4-Iodopyrazole | HCID 77022 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | methyl 3-(4-iodo-1H-pyrazol-1-yl)propanoate | HCID 64435500 | — |
反応手順
To a mixture of 4-iodopyrazole (1.000 g, 5.155 mmol), Cs2CO3 (2.016 g, 6.186 mmol), and DMF (20 mL, 0.2 mol) was added methyl 3-chloropropanoate (758.1 mg, 6.186 mmol) at 0° C. The reaction was heated to 50° C. for 1 h. The material was transferred to a separatory funnel, diluted with EtOAc, and washed with water several times to remove DMF. The organic layer was dry-loaded onto silica gel, and column chromatography was used for purification, eluting with 3:1 Hexanes/EtOAc, affording the title compound as a clear liquid. MS (ES+): m/z=280.95 (100) [MH+]. HPLC: tR=2.91 min (ZQ3, polar—5 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08178668B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-013d4ab7a0e647519da4711fb98ef0af |
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| 出典メモ | uspto-grants-2012_05 |
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