関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 5-Bromopyrimidine-2-carbonitrile | HCID 686546 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 生成物 | 1-(5-Bromopyrimidin-2-yl)ethan-1-one | HCID 53488064 | 61% |
反応手順
To a solution of 5-bromopyrimidine-2-carbonitrile (221 mg, 1.2 mmol) in THF (10 ml) was added methylmagnesium bromide (3.0 ml, 4.20 mmol, 1.4 molar, THF) at −78° C. under nitrogen. The solution was stirred at −78° C. for 3.5 hours, and then quenched with satd aq NH4Cl, and extracted with EtOAc. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. The reaction was purified by column chromatography on silica gel (petroleum ether: EtOAc=1:0 to 0:1) to afford 1-(5-bromopyrimidin-2-yl)ethanone (1.55 mg, 61% yield). 1H NMR (CDCl3 500 MHz): δ 9.00 (s, 2H), 2.80 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09108938B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-71a37e665ded4f3a9f8e1cbfe2daea43 |
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| 出典メモ | uspto-grants-2015_08 |
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