関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | N-methoxy-N-methyl-2-(thiophen-3-yl)acetamide | HCID 11423995 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Phenyl-2-(thiophen-3-yl)ethanone | HCID 12233113 | 55% |
反応手順
To the solution of bromo-benzene (1.0 g, 6.36 mmol) in anhydrous THF (30 mL) was added n-BuLi (5.9 mmol, 2.4 mL) at −78° C. under nitrogen, and the mixture was stirred at −78° C. for further 20 min., a solution of N-methoxy-N-methyl-2-(thiophen-3-yl)acetamide (1 g, 5.4 mmol) in anhydrous THF (10 mL) was added. The resulting mixture was stirred at −78° C. under nitrogen for about 30 min., poured into NH4Cl aqueous solution, and extracted with EtOAc. The organic layers were washed with brine, dried over sodium sulfate, concentrated, and purified by column chromatograph (PE:EtOAc=20:1) to afford Intermediate 2 as a colorless oil (600 mg, yield 55.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09283229B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-3267aa9ccfab4d218c0f17036445456e |
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| 出典メモ | uspto-grants-2016_03 |
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