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Water → Methyl 3-[(cyanomethyl)amino]-4-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromoacetonitrile | HCID 11534 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methyl 3-amino-4-methylbenzoate | HCID 337778 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 3-[(cyanomethyl)amino]-4-methylbenzoate | HCID 86663236 | — |
反応手順
To a stirred solution of 3-amino-4-methyl-benzoic acid, methyl ester (10.0 g) in dry tetrahydrofuran was added N,N-diisopropylethylamine (12.6 mL) followed by the addition of bromoacetonitrile (5.1 mL). The reaction was heated at reflux under an atmosphere of nitrogen with stirring for 12 h. Water was added and the mixture extracted with ethyl acetate. The pooled organics were washed with brine, dried (MgSO4), filtered and the solvent removed under reduced pressure to afford the subtitle compound as a solid (12.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889692B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-d4188331ee3846b4b114635ecbbc573a |
| 出典メモ | uspto-grants-2014_11 |