関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | methyl 1H-indole-5-carboxylate | HCID 2737635 | — |
| 反応物 | 1,1-Difluoro-2-iodoethane | HCID 3833565 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 59625674 | HCID 59625674 | — |
反応手順
To a suspension of NaH (60% dispersion in mineral oil, 59 mg, 1.48 mmol) in DMF (2 mL) was slowly added a solution of 1H-indole-5-carboxylic acid methyl ester 19a (200 mg, 1.14 mmol) in DMF (1 mL) at 0° C. The resulting solution was stirred at 0° C. for 20 min and 1,1-difluoro-2-iodoethane 23a (263 mg, 1.37 mmol) was added. The reaction was warmed to room temperature and stirred for 2 h. The reaction was quenched with water and extracted with EtOAc. The organic layer was concentrated and purified by flash column chromatography (silica gel, 20% EtOAc/hexanes) to afford compound 23b.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748417B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-8e201d7d630d40bb9bc71292aad00fd1 |
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| 出典メモ | uspto-grants-2014_06 |
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