참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-(4-Bromo-2-fluorophenyl)acetonitrile | HCID 7172308 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-(4-Bromo-2-fluorophenyl)-2-methylpropanenitrile | HCID 53403618 | — |
반응 단계
To a slurry of sodium hydride (60% dispersion in mineral oil, 0.82 g, 20.6 mmol) in DMF (20 mL) cooled to 0° C. was added a solution of (4-bromo-2-fluoro-phenyl)-acetonitrile (2.0 g, 9.35 mmol) from Step 1 above, dissolved in THF (10 mL). The reaction was stirred till gas evolution ceased, and then iodomethane (1.3 mL, 20.6 mmol) was added slowly. The reaction was stirred for 30 minutes, and then diluted with 100 mL EtOAc. The solids were removed by filtration, and the organic layer was washed with 100 mL water. The organic layer was dried over MgSO4, and then filtered. The mother liquor was concentrated by rotary evaporation, and the product was distilled under high vacuum (0.3 torr, 45° C.). Yield: 2.25 g, 99%. %. 1H NMR (CDCl3) δ: 2.81 (s, 3H), 2.88 (s, 3H), 7.20-7.25 (m, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07622605B2 |
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| 출처 데이터셋 | uspto-grants-2009_11 |
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| ORD ID | ord-a332514cd04c47be86e11e46b9dffb64 |
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| 출처 메모 | uspto-grants-2009_11 |
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