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Sodium hydride → 1-(2,4-Dimethylbenzyl)-3-methyl-5-nitropyridin-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Methyl-5-nitro-2-pyridone | HCID 89097 | — |
| 反応物 | 1-(Bromomethyl)-2,4-dimethylbenzene | HCID 2734604 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2,4-Dimethylbenzyl)-3-methyl-5-nitropyridin-2(1H)-one | HCID 67267743 | 34% |
反応手順
To a solution containing 0.20 g (1.3 mmol) of 3-methyl-5-nitropyridine-2(1H)-one in 5 ml of N,N-dimethylformamide under a nitrogen atmosphere was added 0.037 g (1.6 mmol) of sodium hydride followed by 0.31 g (1.6 mmol) of 1-bromomethyl-2,4-dimethylbenzene. The reaction was allowed to stir at room temperature for 30 min., quenched with water and extracted with ethyl acetate. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 25% ethyl acetate/hexanes gave 0.12 g (34%) of compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07897607B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-5499473fac7046febb2700c5e56811d0 |
| 出典メモ | uspto-grants-2011_03 |