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Methylamine → 3-(Methylaminomethyl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Benzonitrile, 3-(bromomethyl)- | HCID 97249 | — |
| 生成物 | 3-(Methylaminomethyl)benzonitrile | HCID 457595 | 82% |
反応手順
To a stirred solution of methylamine (40% in water) (200 mL) under N2, was added 3-(bromomethyl)benzonitrile (10 g, 0.051 mol) slowly in small portions over a period of 10 min at 0° C. After being stirred at RT for 3 h, the reaction mixture was extracted with DCM. Then the organic layer was washed with brine and dried over sodium sulphate and concentrated under reduced pressure. The obtained crude was purified using column chromatography on silica gel (pet ether/ethyl acetate) to afford the title compound as a pale yellow liquid (6.1 g, 82%). 1H NMR (DMSO-d6, 400 MHz) δ 7.74 (s, 1H), 7.63-7.68 (m, 2H), 7.48-7.52 (m, 1H) 3.66 (s, 2H), 2.22 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202865B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-0628b36258034376bf59d4f88aa83695 |
| 出典メモ | uspto-grants-2012_06 |